CN108383523B - Dielectric ceramic material - Google Patents
Dielectric ceramic material Download PDFInfo
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- CN108383523B CN108383523B CN201810254627.8A CN201810254627A CN108383523B CN 108383523 B CN108383523 B CN 108383523B CN 201810254627 A CN201810254627 A CN 201810254627A CN 108383523 B CN108383523 B CN 108383523B
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Abstract
The invention relates to a dielectric ceramic material which comprises the following components in parts by weight: 100-120 parts of zirconium oxide; 1-6 parts of a barium titanate composition; 10-20 parts of a binder; 0-5 parts of a plasticizer; the barium titanate composition is a mixture of barium titanate, magnesium oxide and calcium oxide. According to the dielectric ceramic material, after the barium titanate is doped with the magnesium oxide and the calcium oxide, the Curie temperature of the dielectric ceramic material is moved to a high temperature, the temperature reaches about 190 ℃, the Curie peak is expanded, the dielectric constant of the dielectric ceramic material is improved, and the properties such as fracture toughness, bending strength, wear resistance and hardness are good; compared with sapphire, the dielectric ceramic material has the advantages of simple components, low cost, easiness in preparation and processing, reduction in production cost, uniformity and compactness in material, and good wear resistance and dielectric constant without coating or coating.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a dielectric ceramic material.
Background
With the development of electronic product security technology, more and more electronic products have a fingerprint identification function, especially smart phones which are used daily. As fingerprint identification module for cell-phone, need to have sensitive fingerprint identification speed and wearability. Traditional fingerprint identification module is mostly capacitanc fingerprint identification chip, and the dielectric cover plate of this chip mainly is made by sapphire, glass etc.. However, the cost of sapphire is high, the dielectric constant is not ideal (the dielectric constant of sapphire is 9-11), and the hardness is too high, so that the processing is difficult and the production cost is high. The glass dielectric cover plate has the problems of poor wear resistance, low strength, low dielectric constant and the like, and aiming at the problems, the problems of poor wear resistance and low dielectric constant are solved by adopting a coating film, a coating layer and the like, but the problems of poor binding force between materials and the like are caused due to the difference of thermal expansion coefficients of the coating layer and the coating layer.
Disclosure of Invention
Based on the above, the invention provides a dielectric ceramic material which has the characteristics of higher dielectric constant and good wear resistance, and compared with sapphire, the dielectric ceramic material has the advantages of lower cost and easy processing.
A dielectric ceramic material comprises the following components in parts by weight:
the barium titanate composition is a mixture of barium titanate, magnesium oxide and calcium oxide.
After the barium titanate is doped with the magnesium oxide and the calcium oxide, the Curie temperature of the dielectric ceramic material is shifted to high temperature, reaches about 190 ℃, the Curie peak is expanded, the dielectric constant of the dielectric ceramic material is improved, and the properties such as fracture toughness, bending strength, wear resistance and hardness are good; compared with sapphire, the dielectric ceramic material has the advantages of simple components, low cost, easiness in preparation and processing, reduction in production cost, uniformity and compactness in material, and good wear resistance and dielectric constant without coating or coating.
In one embodiment, the dielectric ceramic material comprises the following components in parts by weight:
in one embodiment, the molar ratio of barium titanate, magnesium oxide and calcium oxide is 10-20: 2-3: 0.8 to 1.5.
In one embodiment, the barium titanate composition is prepared by: mixing a titanium tetrachloride solution and a refined barium chloride solution, and adding oxalic acid (the molar ratio is TiCl) at 70-100 DEG C4：BaC12：H2C2O4·2H2O is 1: 1: 2) reacting to generate a barium titanyl oxalate precipitate, adding magnesium hydroxide and calcium hydroxide, uniformly mixing, filtering, washing, drying, calcining at 700-1000 ℃, and screening to obtain the barium titanate composition.
In one embodiment, the barium titanate composition has a barium titanate content of 85% by mass or more.
In one embodiment, the barium titanate composition has a particle size of 0.8 to 2 μm.
In one embodiment, the zirconia is yttrium stabilized zirconia.
In one embodiment, the binder is polyvinyl alcohol with a mass content of 5%, and the plasticizer is DBP and/or DOP.
In one embodiment, the binder comprises the following components in parts by weight:
in one embodiment, the vinyl acetate in the ethylene-vinyl acetate copolymer accounts for 16-20% of the weight of the ethylene-vinyl acetate copolymer.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The invention provides a dielectric ceramic material which can be used for preparing elements such as a fingerprint identification cover plate and the like, is sensitive in reaction and comprises the following components in parts by weight:
in some embodiments, the dielectric ceramic material comprises the following components in parts by weight:
the barium titanate composition is a mixture of barium titanate, magnesium oxide and calcium oxide, and the mass content of barium titanate in the barium titanate composition is more than or equal to 85%. Oxygen gasDoping of magnesium oxide and calcium oxide into barium titanate, Ca2+、Mg2+Substituted moiety Ba2+And part of axes in the crystal structure is lengthened, so that the crystal structure is asymmetric and is easier to polarize, and the coercive field strength is reduced. Preferably, the molar ratio of barium titanate, magnesium oxide and calcium oxide is 10-20: 2-3: 0.8 to 1.5.
The preparation method of the barium titanate composition comprises the following steps: mixing a titanium tetrachloride solution and a refined barium chloride solution, and adding oxalic acid (the molar ratio is TiCl) at 70-100 DEG C4：BaC12：H2C2O4·2H2O is 1: 1: 2) and (3) carrying out reaction to generate a barium titanyl oxalate precipitate, wherein the molar ratio of barium titanate to magnesium oxide to calcium oxide is 10-20: 2-3: 0.8-1.5, adding corresponding amount of magnesium hydroxide and calcium hydroxide (the molar weight of the magnesium hydroxide is equal to that of the magnesium oxide, and the molar weight of the calcium hydroxide is equal to that of the calcium oxide) into the barium titanyl oxalate precipitate, uniformly mixing, filtering, washing, drying, calcining at 700-1000 ℃, screening, and taking the barium titanate composition with the granularity of 0.8-2 mu m.
The granularity of the barium titanate composition is 0.8-2 mu m, and when the granularity of the barium titanate composition is less than 0.8 mu m, the flowability of the particles is poor, so that the particles are not beneficial to uniform mixing; when the particle size of the barium titanate composition is larger than 2 μm, barium titanate is easily agglomerated and is not favorable for compact molding.
In some embodiments, the zirconia is yttrium stabilized zirconia.
When the tape casting method is used for molding, preferably, the binder is polyvinyl alcohol with a mass content of 5%, and the plasticizer is DBP (Dibutyl Phthalate) and/or DOP (Dioctyl Phthalate).
When the injection molding method is adopted for molding, the adhesive is a composition comprising the following components in parts by weight:
the adhesive can enable a ceramic body to be more tightly adhered in the forming process, the probability of generating pores in the ceramic body after glue discharging is reduced, the ethylene-vinyl acetate copolymer reduces the crystallinity of the adhesive, the adhesive can be degreased more quickly at a lower temperature during thermal degreasing, the random polypropylene is used as a flowing agent and a dispersing agent, the fluidity of the adhesive is adjusted, the fluidity and the dispersibility of the adhesive are good during application, the adhesive is uniformly mixed with ceramic powder, the ceramic body is uniformly formed and has consistent properties, and the problems of collapse, foaming, deformation or cracking caused by unbalanced tension due to non-uniform body are avoided.
Preferably, the vinyl acetate in the ethylene-vinyl acetate copolymer accounts for 16-20% of the weight of the ethylene-vinyl acetate copolymer, so that the effect of better increasing the toughness and the impact resistance of the ceramic blank is achieved.
The coupling agent is stearic acid and/or ester derivatives thereof, wherein the ester derivatives can be butyl stearate and/or octyl stearate.
According to the dielectric ceramic material, after the barium titanate is doped with the magnesium oxide and the calcium oxide, the Curie temperature of the dielectric ceramic material is moved to a high temperature, the temperature reaches about 190 ℃, the Curie peak is expanded, the dielectric constant of the dielectric ceramic material is improved, and the properties such as fracture toughness, bending strength, wear resistance and hardness are good; compared with sapphire, the dielectric ceramic material has the advantages of simple components, low cost, easiness in preparation and processing, reduction in production cost, uniformity and compactness in material, and good wear resistance and dielectric constant without coating or coating.
Example 1
The dielectric ceramic material of the embodiment is used for preparing a fingerprint identification cover plate. The dielectric ceramic material comprises the following components in parts by weight:
the barium titanate composition is a mixture of barium titanate, magnesium oxide and calcium oxide, and the molar ratio of barium titanate, magnesium oxide and calcium oxide is 20: 3: 0.8.
the preparation method of the barium titanate composition comprises the following steps: dissolving titanium tetrachloride solution and refined barium chloride solutionMixing the solutions, adding oxalic acid (molar ratio is TiCl) at 80 deg.C4：BaC12：H2C2O4·2H2O is 1: 1: 2) reacting to generate a barium titanyl oxalate precipitate, wherein the molar ratio of barium titanate to magnesium oxide to calcium oxide is 20: 3: 0.8, adding magnesium hydroxide and calcium hydroxide with corresponding amount into the barium titanyl oxalate precipitate, uniformly mixing, filtering, washing, drying, calcining at 850 ℃, and screening to obtain the barium titanate composition with the granularity of 0.8-2 mu m.
The zirconia is yttrium stabilized zirconia.
The adhesive is polyvinyl alcohol with the mass content of 5%, and the plasticizer is DBP.
The dielectric ceramic material is prepared into the fingerprint identification cover plate by adopting a tape casting forming method, and the method comprises the following steps: step 1: the following components are taken according to parts by weight: 100 parts of zirconium oxide, 1.5 parts of barium titanate composition, 15 parts of binder and 5 parts of plasticizer, fully mixing the zirconium oxide, the barium titanate composition, the dispersant and the solvent, sequentially adding the binder and the plasticizer, and uniformly mixing to obtain a mixed raw material; the dispersing agent is 4 parts by weight of triolein, the solvent is 40 parts by weight of a mixture of isobutanol and ethyl acetate, and the volume ratio of the isobutanol to the ethyl acetate is 1: 3.
Step 2: adding the mixed raw materials into a high-pressure dispersion machine, and mixing the raw materials by the high-pressure dispersion machine to obtain fully-dispersed slurry for tape casting;
and step 3: defoaming the completely dispersed slurry for tape casting to obtain defoamed slurry;
and 4, step 4: carrying out tape casting on the defoamed slurry, and then carrying out sectional drying, wherein the drying temperature of a first section is 60 ℃, the drying temperature of a second section is 85 ℃, and the drying temperature of a third section is 100 ℃ to obtain a green body;
and 5: punching the green body, and then discharging the glue to obtain a green body after glue discharging;
step 6: sintering the green body after the binder removal at a high temperature, and naturally cooling the green body along with a furnace to obtain a biscuit;
and 7: and mechanically grinding the biscuit, and then polishing to enable the fingerprint identification cover plate to have a mirror surface effect.
Example 2
The dielectric ceramic material of the embodiment is used for preparing a fingerprint identification cover plate. The dielectric ceramic material comprises the following components in parts by weight:
105 parts of zirconium oxide;
2 parts of a barium titanate composition;
12 parts of a binder.
The barium titanate composition is a mixture of barium titanate, magnesium oxide and calcium oxide, and the molar ratio of the barium titanate, the magnesium oxide and the calcium oxide is 18:2.8: 1.
The preparation method of the barium titanate composition comprises the following steps: mixing titanium tetrachloride solution and refined barium chloride solution, adding oxalic acid (molar ratio is TiCl) at 85 deg.C4：BaC12：H2C2O4·2H2O is 1: 1: 2) reacting to generate a barium titanyl oxalate precipitate, adding corresponding amount of magnesium hydroxide and calcium hydroxide into the barium titanyl oxalate precipitate according to the molar ratio of the barium titanate to the magnesium oxide to the calcium oxide of 18:2.8:1, uniformly mixing, filtering, washing, drying, calcining at 900 ℃, and screening to obtain the barium titanate composition with the granularity of 0.8-2 mu m.
The zirconia is yttrium stabilized zirconia.
The adhesive is a composition comprising the following components in parts by weight:
the vinyl acetate in the ethylene-vinyl acetate copolymer accounts for 16-20% of the weight of the ethylene-vinyl acetate copolymer.
The coupling agent is octyl stearate.
The fingerprint identification cover plate is made of the dielectric ceramic material by an injection molding method, and comprises the following steps:
step 1: taking 43 parts of paraffin wax, 6.5 parts of microcrystalline wax, 8 parts of high-density polyethylene, 8 parts of ethylene-vinyl acetate copolymer, 5 parts of atactic polypropylene and 2 parts of coupling agent by weight parts, uniformly mixing at a preset temperature, discharging and cooling to obtain a binder;
step 2: taking 105 parts of zirconium oxide and 2 parts of barium titanate composition according to parts by weight, and mixing a binder with the zirconium oxide and barium titanate composition to obtain a feed;
and step 3: injection molding the feed to obtain a green body;
and 4, step 4: degreasing the green body by using a solvent, thermally degreasing and sintering, and naturally cooling along with a furnace to obtain a biscuit;
and 5: and mechanically grinding the biscuit, and then polishing to enable the fingerprint identification cover plate to have a mirror surface effect.
Example 3
The dielectric ceramic material of the embodiment is used for preparing a fingerprint identification cover plate. The dielectric ceramic material comprises the following components in parts by weight:
the barium titanate composition is a mixture of barium titanate, magnesium oxide and calcium oxide, and the molar ratio of the barium titanate, the magnesium oxide and the calcium oxide is 15:2.5: 1.5.
The preparation method of the barium titanate composition comprises the following steps: mixing titanium tetrachloride solution and refined barium chloride solution, adding oxalic acid (molar ratio is TiCl) at 100 deg.C4：BaC12：H2C2O4·2H2O is 1: 1: 2) reacting to generate a barium titanyl oxalate precipitate, adding corresponding amount of magnesium hydroxide and calcium hydroxide into the barium titanyl oxalate precipitate according to the molar ratio of the barium titanate to the magnesium oxide to the calcium oxide of 15:2.5:1.5, uniformly mixing, filtering, washing, drying, calcining at 1000 ℃, and screening to obtain the barium titanate composition with the granularity of 0.8-2 mu m.
The zirconia is yttrium stabilized zirconia.
The adhesive is polyvinyl alcohol with the mass content of 5 percent, and the plasticizer is DOP.
The manufacturing method of the fingerprint identification cover plate of the embodiment is the same as that of the embodiment 1.
Example 4
The dielectric ceramic material of the embodiment is used for preparing a fingerprint identification cover plate. The dielectric ceramic material comprises the following components in parts by weight:
the barium titanate composition is a mixture of barium titanate, magnesium oxide and calcium oxide, and the molar ratio of the barium titanate to the magnesium oxide to the calcium oxide is 10:2: 1.2.
The preparation method of the barium titanate composition comprises the following steps: mixing titanium tetrachloride solution and refined barium chloride solution, adding oxalic acid (molar ratio is TiCl) at 90 deg.C4：BaC12：H2C2O4·2H2O is 1: 1: 2) reacting to generate a barium titanyl oxalate precipitate, adding corresponding amount of magnesium hydroxide and calcium hydroxide into the barium titanyl oxalate precipitate according to the molar ratio of the barium titanate to the magnesium oxide to the calcium oxide of 10:2:1.2, uniformly mixing, filtering, washing, drying, calcining at 1000 ℃, and screening to obtain the barium titanate composition with the granularity of 0.8-2 mu m.
The zirconia is yttrium stabilized zirconia.
The adhesive is a composition comprising the following components in parts by weight:
preferably, the ethylene-vinyl acetate copolymer comprises 20% by weight of vinyl acetate based on the weight of the ethylene-vinyl acetate copolymer.
The manufacturing method of the fingerprint identification cover plate of the embodiment is the same as that of the embodiment 2.
Example 5
The dielectric ceramic material of the embodiment is used for preparing a fingerprint identification cover plate. The dielectric ceramic material comprises the following components in parts by weight:
the barium titanate composition is a mixture of barium titanate, magnesium oxide and calcium oxide, and the molar ratio of the barium titanate, the magnesium oxide and the calcium oxide is 12:2.2: 1.
The preparation method of the barium titanate composition comprises the following steps: mixing titanium tetrachloride solution and refined barium chloride solution, adding oxalic acid (molar ratio is TiCl) at 80 deg.C4：BaC12：H2C2O4·2H2O is 1: 1: 2) reacting to generate a barium titanyl oxalate precipitate, adding corresponding amount of magnesium hydroxide and calcium hydroxide into the barium titanyl oxalate precipitate according to the molar ratio of the barium titanate to the magnesium oxide to the calcium oxide of 12:2.2:1, uniformly mixing, filtering, washing, drying, calcining at 950 ℃, and screening to obtain the barium titanate composition with the granularity of 0.8-2 mu m.
The zirconia is yttrium stabilized zirconia.
When the injection molding method is adopted for molding, the adhesive is a composition comprising the following components in parts by weight:
the vinyl acetate in the ethylene-vinyl acetate copolymer accounts for 18 percent of the weight of the ethylene-vinyl acetate copolymer.
The manufacturing method of the fingerprint identification cover plate of the embodiment is the same as that of the embodiment 2.
Comparative example 1
The dielectric ceramic material of the present comparative example was prepared in the same manner as in example 3, except that the barium titanate composition was replaced with barium titanate, and the fingerprint identification cover plate was prepared from the dielectric ceramic material of the present comparative example by a tape casting method in the same manner as in example 3.
The fingerprint identification covers prepared in examples 1 to 5 and comparative example 1 were measured for dielectric constant, Vickers strength, room temperature bending strength and room temperature fracture toughness, and the results are shown in Table 1.
TABLE 1
From the above test results, it can be seen that the fingerprint identification cover plates of examples 1 to 5 using the dielectric ceramic material of the present invention have significantly improved dielectric constant, vickers strength, room temperature bending strength, and room temperature fracture toughness in all aspects relative to the fingerprint identification cover plate of comparative example 1, and the molar ratio of barium titanate, magnesium oxide, and calcium oxide in barium titanate is 10-20: 2-3: 0.8 to 1.5 of magnesium oxide and calcium oxide are doped, and the doped magnesium oxide and calcium oxide are applied to the dielectric ceramic material, so that the dielectric constant of the dielectric ceramic material is effectively improved, and the material also contributes to improving the strength, bending resistance and toughness of the material.
The dielectric constant of the dielectric ceramic material is 3-4 times of that of sapphire, the bending resistance and the toughness of the dielectric ceramic material are better than those of sapphire, the dielectric ceramic material is not easy to crack, the cost of the material is much lower than that of sapphire, the dielectric ceramic material is easy to prepare and process, and the production cost is reduced.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. The dielectric ceramic material is characterized by comprising the following components in parts by weight:
the barium titanate composition is a mixture of barium titanate, magnesium oxide and calcium oxide;
the molar ratio of the barium titanate, the magnesium oxide and the calcium oxide is (10-20) to (2-3): (0.8 to 1.5).
2. The dielectric ceramic material of claim 1, wherein the dielectric ceramic material is composed of the following components in parts by weight:
3. a dielectric ceramic material according to claim 1 or 2, characterized in that the barium titanate composition is prepared by a process comprising: mixing a titanium tetrachloride solution and a refined barium chloride solution, and adding oxalic acid (the molar ratio is TiCl) at 70-100 DEG C4：BaC12：H2C2O4·2H2O is 1: 1: 2) reacting to generate a barium titanyl oxalate precipitate, adding magnesium hydroxide and calcium hydroxide, uniformly mixing, filtering, washing, drying, calcining at 700-1000 ℃, and screening to obtain the barium titanate composition.
4. A dielectric ceramic material according to claim 1 or 2, wherein the mass content of barium titanate in the barium titanate composition is not less than 85%.
5. A dielectric ceramic material according to claim 1 or 2, wherein the barium titanate composition has a particle size of 0.8 to 2 μm.
6. A dielectric ceramic material according to claim 1 or 2, wherein the zirconia is yttrium-stabilized zirconia.
7. A dielectric ceramic material according to claim 1 or 2, wherein the binder is polyvinyl alcohol with a mass content of 5%, and the plasticizer is DBP and/or DOP.
8. A dielectric ceramic material according to claim 1 or 2, wherein the binder comprises the following components in parts by weight:
9. the dielectric ceramic material of claim 8, wherein the vinyl acetate in the ethylene-vinyl acetate copolymer accounts for 16-20% of the weight of the ethylene-vinyl acetate copolymer.
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