CN117923892A - Anti-reduction X7R type superfine ceramic material and preparation method thereof - Google Patents
Anti-reduction X7R type superfine ceramic material and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 26
- 239000000654 additive Substances 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 22
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 20
- 230000000996 additive effect Effects 0.000 claims abstract description 14
- 239000012298 atmosphere Substances 0.000 claims abstract description 13
- 238000010405 reoxidation reaction Methods 0.000 claims abstract description 13
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 7
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 7
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 20
- 238000000498 ball milling Methods 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 13
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 229910052573 porcelain Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000011805 ball Substances 0.000 claims 2
- 238000009413 insulation Methods 0.000 abstract description 11
- 229910002113 barium titanate Inorganic materials 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 4
- 239000012776 electronic material Substances 0.000 abstract description 2
- 239000003985 ceramic capacitor Substances 0.000 description 14
- 230000008859 change Effects 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 11
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 9
- 239000003990 capacitor Substances 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- 239000003989 dielectric material Substances 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000010953 base metal Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229910011763 Li2 O Inorganic materials 0.000 description 1
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- -1 adds Bi 2O3 Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
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Abstract
An anti-reduction X7R type superfine ceramic material and a preparation method thereof belong to the technical field of electronic materials, and in particular relate to the ceramic material technology. The anti-reduction X7R superfine ceramic material consists of BaTiO 3 with the main material particle size of 100-200 nm and a secondary additive; the secondary additive comprises ZrO 2、BaCO3、WO3、Mn3O4 and one or more oxides of rare earth elements Y, dy, ho, er; the mass ratio of each material is ：[100-(a+b+c+d+e)]BaTiO3+aBaCO3+bZrO2+cWO3+dMn3O4+eRe2O3,Re2O3 to represent rare earth element oxide, wherein a, b, c, d, e is a coefficient, and the weight percentage of the material is 0.4 to 4 percent, 0.1 to 0.4 percent, 0.02 to 0.08 percent, 0.2 to 0.8 percent, and 0.4 to 1.6 percent. The mass of the secondary additive accounts for 1.32-5.68% of the total mass of the whole anti-reduction X7R type superfine ceramic material. The anti-reduction X7R superfine ceramic material is prepared by sintering in 1-2% H 2-N2 reducing atmosphere and performing reoxidation treatment, has high dielectric constant (2000-3000), higher insulation resistivity (rho is more than or equal to 1.0X 10 12 ohm cm), good temperature stability, good repeatability and low price, and can be used for preparing high-performance and low-cost Ni electrode MLCC.
Description
Technical Field
The invention belongs to the technical field of electronic materials, and relates to a ceramic material and a preparation method thereof.
Background
Ceramic capacitors are classified into thin film capacitors, wafer capacitors, multilayer ceramic capacitors, barrier layer capacitors, and the like in terms of element forms.
With rapid development of consumer electronics and industrial intelligence in recent years, vigorous development of passive devices including multilayer ceramic capacitors (Multilayer Ceramic Capacitors, MLCC) is promoted, and the multilayer ceramic capacitors are monolithic capacitor devices which are formed by alternately stacking ceramic dielectrics and metal inner electrodes, sintering the ceramic dielectric and the metal inner electrodes together, coating terminal electrodes at two ends of the ceramic dielectric and the metal inner electrodes, and packaging the ceramic dielectric and the metal inner electrodes. Compared with a capacitor with a common structure, the MLCC has the advantages of small volume, large specific volume, small equivalent series resistance ESR, good moisture resistance, high reliability, capability of effectively reducing the volume and weight of electronic information terminal products (especially portable products), improving the reliability of the products and the like, and conforms to the development direction of miniaturization, light weight, high performance and multifunction of the IT industry.
The ceramic capacitor is classified into a type I ceramic capacitor and a type II ceramic capacitor according to the temperature characteristics of the ceramic medium. The class I ceramic capacitor has small capacity, low loss, good temperature stability and linear change of dielectric constant along with temperature, and is commonly used for compensation circuits, high-frequency circuits and the like; the type II ceramic capacitor has poor capacity response and temperature stability, and the dielectric constant changes nonlinearly and is commonly used for a coupling circuit, a smoothing circuit and the like. According to the international electronic industry association (Electronic Industries Association, EIA) standard, the temperature characteristics of a class II ceramic capacitor consist of three parts, representing the minimum temperature, the maximum temperature and the maximum deviation of the allowable capacitance with temperature change (taking the capacitance of 25 ℃ as a reference value), respectively. The X7R type ceramic material is a ceramic material with a temperature range of-55-125 ℃ and a capacity temperature change rate (TCC) of less than +/-15 percent.
The types of the inner electrode materials of the MLCC can be classified into a noble metal inner electrode (Prexious Metal Electrode) multilayer ceramic capacitor (PME-MLCC) and a base metal inner electrode (Basw Metal Electrode) multilayer ceramic capacitor (BME-MLCC). The PME-MLCC is sintered in air using noble metals such as Pb, ag, etc. as internal electrodes. The BME-MLCC adopts Cu and Ni which are relatively low in price as the inner electrodes. Meanwhile, the Ni electrode has unique advantages, such as lower resistivity than Pd and Ag70-Pd30 electrodes, and is beneficial to reducing ESR; the electromigration rate is low, and the electrochemical stability is good; the reliability of the connection of the Ni inner electrode and the Ni outer electrode is high; the mechanical strength of the Ni-MLCC is high, and the flexural strength is high; the melting point is higher than Cu, and the electrode is favorable for sintering the MLCC.
It is worth noting that the internal electrode is easily oxidized and loses conductivity by high-temperature sintering in air, so that the porcelain needs to be sintered in a reducing atmosphere. However, sintering of barium titanate ceramic materials in a reducing atmosphere may cause Ti 4+ to be reduced to Ti 3+, while creating free mobile weakly bound electrons and oxygen vacancies, which may cause n-type semiconducting of the ceramic dielectric material.
In order to solve the problems, in the sixties of the twentieth century, research and development work of barium titanate-based anti-reduction dielectric materials is started by foreign researchers her, and it is found that elements such as Mn, co and Mg are added to barium titanate respectively to replace Ti to form acceptor doping, so that the anti-reduction dielectric material can be obtained. However, acceptor doping alone generates more oxygen vacancies, which worsen electrical performance. In order to eliminate defects such as oxygen vacancies caused by low oxygen partial pressure during sintering, the ceramic is reoxidized at a lower temperature and a slightly higher oxygen partial pressure. At present, the reduction sintering resistance of the alloy is mainly realized in countries and regions with more researches, and the temperature stability is optimized. However, metallic Ta is expensive, li element is volatile, and the dielectric constant of the system is low (epsilon=895). The patent No. 20091010488. X discloses an anti-reduction nickel electrode ceramic dielectric material, wherein a main crystal phase is synthesized by mixing BaO and TiO 2, and a modified additive is one or more of Nb 2O5、Dy2O3、MnO、MgO、CaO、Y2O3. One or more of glass fluxing agents SiO 2、ZnO、Li2 O, baO are added. The dielectric constant of the material reaches 2500-2800, but the insulation resistance of the material is low (2-3 multiplied by 10 10 omega). The university of martial arts, herkuh-Hua et al discloses a preparation method of an anti-reduction BaTiO 3 -based ceramic material, which takes barium titanate as a base material, adds Bi 2O3、ZnO、Y2O3, and carries out sintering under a reducing atmosphere to prepare the anti-reduction BaTiO 3 -based ceramic material with larger dielectric constant change range (700-2000), high insulation resistivity (more than 10 12 ohm cm) at room temperature and temperature stability meeting X8R standard. However, the sintering temperature of the dielectric ceramic material is too high (1300-1480 ℃), and the dielectric constant is not high as a whole, so that the higher requirements cannot be met. Chinese patent number 202110649477.2 discloses a preparation method of an anti-reduction X8R type BaTiO 3 -based ceramic material. BaTiO 3、Bi2O3、MgO、ZrO2 is used as a raw material, and a benign charge compensation mechanism is established by doping and modifying acceptor ions together, so that the barium titanate-based dielectric ceramic material with dielectric constant of 669-2020, insulation resistivity of 1.22-4.84 multiplied by 10 13 ohm cm and temperature stability meeting EIAX7R, X R standard is prepared. But its dielectric constant varies widely and is at most 2020.
High specific volume is one of the most important development trends of MLCC, and the nanocrystallization of dielectric layer powder is a necessary requirement for realizing the thinning of MLCC. The grain diameter of the currently used barium titanate is basically between 200nm and 1000nm, and the invention uses 100nm to 200nm of superfine barium titanate as a base material, and prepares the ceramic material which is anti-reduction, low-loss, high in dielectric constant and insulation resistivity and meets the X7R capacitance temperature coefficient change standard by utilizing an adjustment process and doping ZrO 2、BaCO3、WO3、Mn3O4 and rare earth elements.
Disclosure of Invention
The invention aims to provide a reduction-resistant X7R ultrafine ceramic material which is sintered at medium temperature, resistant to reduction, low in loss, high in dielectric constant, and suitable for a multilayer ceramic capacitor, and a preparation method thereof, wherein the reduction-resistant X7R ultrafine ceramic material meets the temperature coefficient change standard of X7R capacitance.
The technical scheme of the invention is as follows:
the medium material takes ultrafine porcelain material BaTiO 3 with the grain diameter of 100 nm-200 nm as a main material, which accounts for 94.32-98.68 percent of the total weight of the medium material, and various secondary additives are added, which accounts for 1.32-5.68 percent of the total weight of the medium material, so as to prepare the anti-reduction X7R ultrafine ceramic material.
The invention provides an anti-reduction X7R type superfine ceramic material, which is characterized in that: the medium material consists of main materials of 100-200 nm of ultrafine BaTiO 3 and secondary additives; the secondary additive comprises ZrO 2、BaCO3、WO3、Mn3O4 and one or more oxides of rare earth elements Y, dy, ho, er. Wherein the secondary additives account for the total mass of the ceramic material in percentage ZrO2：0.1～0.4％、BaCO3：0.4～4％、WO3：0.02～0.08％、Mn3O4：0.2～0.8％、Re2O3：0.4～1.6％.
The dielectric constant of the ceramic material is between 2000 and 3000, the dielectric loss is less than 2.5 percent, and the capacity temperature change rate is < +/-15 percent, so that the ceramic material is a dielectric ceramic material meeting the X7R standard.
The preparation method of the ceramic material is characterized by comprising the following steps:
Step 1: ball-milling and mixing ultrafine BaTiO 3 powder with the particle size of 100-200 nm and one or more modified additives selected from ZrO 2、BaCO3、WO3、Mn3O4 and rare earth oxides uniformly, granulating and forming to obtain a green blank; wherein the addition amount of the modifying additive accounts for 1.32-5.68% of the mass sum of the main crystal phase powder and the modifying additive;
Step 2: sintering; sintering the green body obtained in the step 1 for 2-4 hours at 1300-1350 ℃ in a mixed reducing atmosphere of 1-2% H 2-N2;
Step 3: reoxidation; and (3) carrying out reoxidation treatment on the sample obtained in the step (2) for 2 hours under the protection of N 2 atmosphere containing O 2 at the temperature of 900-1100 ℃ to obtain the final anti-reduction X7R superfine ceramic material.
The ball milling process in the step 1 is as follows: using zirconium dioxide balls as ball milling medium, deionized water as solvent, ball milling for 3-16 hours according to the weight ratio of 1:3-5:0.5-1;
the granulation process in the step 1 is as follows: drying the ball-milling mixture, mixing the ball-milling mixture with a polyvinyl alcohol aqueous solution, granulating, and controlling the granulating size to be 80-250 meshes;
the molding process in the step 1 is as follows: putting the pelleting material into a forming die, and performing dry press forming under the pressure of 10MPa to obtain a raw blank;
The reoxidation process in step 3 is as follows: the oxygen content in the N 2 atmosphere containing O 2 is 10-200 ppm.
The invention provides (prepared) an anti-reduction X7R superfine ceramic material, which is different from MnCO 3 commonly used in the prior patent by adopting an additive Mn 3O4 and has the following action mechanism: the valence-changing mechanism of the atmosphere to Ti 4+ ions is influenced by the characteristics of the 3d transition metal element in a polyvalent state. Mn ions in Mn 3O4 have valence states of Mn 3+ and Mn 2+, mn ions with valence of +3 are reduced to valence of +2 under the influence of a reducing atmosphere, ti 4+ ions are prevented from being converted into Ti 3+ ions, and the reduction resistance of the material is enhanced. The co-doping mechanism of the additive rare earth oxide Re 2O3 and Mn 3O4 is as follows: according to the Kroger-Vink defect equation, mn 3+ ions are reduced to Mn 2+ ions during sintering to produceThe defect dipole inhibits electron length Cheng Yue migration, ensures that barium titanate is not subjected to N-type semi-conduction, enhances dielectric relaxation, improves temperature stability to some extent, and can keep good insulation property.
The anti-reduction X7R superfine ceramic material provided by the invention has lower dielectric loss (tg delta is less than or equal to 2.5%), higher insulation resistivity (rho is more than or equal to 1.0X 10 12 omega cm), capacitance temperature coefficient meeting X7R standard, higher dielectric constant (2000-3000) and good processability through test. The preparation process is basically the same as the traditional production process except that the sintering is carried out in a mixed reducing atmosphere. The method is shown to be capable of preparing the anti-reduction X7R superfine ceramic material with compact structure, good processability, lower dielectric loss, high dielectric constant and higher insulation resistivity.
Compared with the prior art, the invention has the following characteristics:
1. In the formula, the content of Zr 2+、W6+、Mn3+、Mn2+ and other rare earth element doped ions is controlled by comprehensively regulating a, b, c, d, e values, so that the aims of synthesizing the anti-reduction porcelain by regulating the stoichiometric ratio and improving the formula and realizing the comprehensive regulation of dielectric properties are fulfilled.
2. In the formula, mn 3O4 is used as a modification additive, mn 3+ is reduced into Mn 2+ in a reducing atmosphere, ti 4+ ions are prevented from being converted into Ti 3+ ions, and the reduction resistance of the porcelain is enhanced; mn 2+ and Ti 4+ The defective dipole enhances temperature stability and enables it to maintain good insulating properties.
3. In the formula, the additive for secondary synthesis is not needed, so that the method is beneficial to industrialized mass production and effectively reduces the complexity of the preparation link.
4. The reoxidation process is adopted, so that the problem that the insulation resistance of the MLCC product is attenuated under direct current bias and the electrical property is deteriorated due to oxygen vacancies formed by Mn valence variation is solved. The reoxidation process (i.e., annealing in a weak oxidizing atmosphere) reduces the mobility of oxygen vacancies and effectively improves the reliability of the MLCC device.
5. The raw materials of the anti-reduction ceramic material prepared by the invention are abundant in China and low in price, and particularly, base metal Ni is adopted to replace precious metals such as Pb, ag and the like as the inner electrode of the MLCC, so that the cost of the MLCC device is greatly reduced, and the low cost of the high-performance MLCC is possible.
Drawings
FIG. 1 is a schematic flow chart of a preparation method of the anti-reduction X7R type ultrafine ceramic material.
FIG. 2 is a TEM image of ultrafine barium titanate raw material particles having a particle diameter of 120.+ -. 20nm used in the present invention.
FIG. 3 is a graph showing the dielectric constant versus temperature of the samples of examples 1-4 of the present invention.
FIG. 4 is a graph showing the temperature change rate of the sample capacitor according to examples 1 to 4 of the present invention.
FIG. 5 is a graph showing the dielectric constant versus temperature of the samples of examples 5-7 of the present invention.
FIG. 6 is a graph showing the temperature change rate of the sample capacitor according to examples 5 to 7 of the present invention.
FIG. 7 is a graph showing the dielectric constant versus temperature of the samples of examples 8-10 of the present invention.
FIG. 8 is a graph showing the temperature change rate of the sample capacitor according to examples 8 to 10 of the present invention.
Detailed Description
Examples 1 to 10
Step 1: batching; the starting materials were weighed exactly in the proportions indicated in table 1.
Step 2: ball milling; ball milling the raw materials prepared in the step1 in deionized water for 16 hours and drying.
Step 3: granulating and molding; adding polyvinyl alcohol into the ball-milling material in the step 2 for granulating, controlling the granulating size to be 80-250 meshes, and pressing the ball-milling material into green bodies under 10 MPa;
Step 4: sintering; sintering the green body obtained in the step 3 for 2-4 hours at the temperature of 1300-1350 ℃ in a reducing atmosphere of 1-2% H 2-N2;
Step 5: reoxidation; and (3) sintering the sample obtained in the step (4) for 2 hours under the protection of N 2 atmosphere (with the oxygen content of 10-200 ppm) containing O 2 at the temperature of 900-1100 ℃ to obtain the final anti-reduction ceramic material, wherein the specific process is shown in Table 2. The results of the performance test (dielectric loss, dielectric constant, insulation resistivity, and temperature change rate of capacitance) of the obtained materials are shown in tables 3 and 4.
TABLE 1 anti-reduction X7R superfine ceramic Material examples 1-10 batching Table
TABLE 2 Table 2 Process of examples 1-10 of anti-reduction X7R ultrafine ceramic materials
| Examples numbering | Sintering temperature | Sintering time | Reoxidation temperature | Reoxidation time | Sintering atmosphere |
| 1 | 1300℃ | 2 | 900℃ | 2 | 1％H2-N2 |
| 2 | 1300℃ | 2 | 900℃ | 2 | 1％H2-N2 |
| 3 | 1300℃ | 2 | 900℃ | 2 | 1％H2-N2 |
| 4 | 1300℃ | 2 | 900℃ | 2 | 1％H2-N2 |
| 5 | 1325℃ | 3 | 1000℃ | 2 | 1.5％H2-N2 |
| 6 | 1325℃ | 3 | 1000℃ | 2 | 1.5％H2-N2 |
| 7 | 1325℃ | 3 | 1000℃ | 2 | 1.5％H2-N2 |
| 8 | 1350℃ | 4 | 1100℃ | 2 | 2％H2-N2 |
| 9 | 1350℃ | 4 | 1100℃ | 2 | 2％H2-N2 |
| 10 | 1350℃ | 4 | 1100℃ | 2 | 2％H2-N2 |
TABLE 3 Table of the Properties of examples 1-10 of anti-reduction X7R ultrafine ceramic materials
| Examples numbering | Sintering temperature-reoxidation temperature | Dielectric loss tgδ (%) | Insulation resistivity ρ (Ω·cm) | Dielectric constant epsilon |
| 1 | 1300℃-900℃ | 2.2 | 1.3*1012 | 2193 |
| 2 | 1300℃-900℃ | 1.4 | 1.9*1012 | 2549 |
| 3 | 1300℃-900℃ | 1.3 | 2.5*1012 | 2717 |
| 4 | 1300℃-900℃ | 1.5 | 2.9*1012 | 2788 |
| 5 | 1325℃-1000℃ | 1.4 | 2.5*1012 | 2213 |
| 6 | 1325℃-1000℃ | 1.6 | 2.6*1012 | 2645 |
| 7 | 1325℃-1000℃ | 1.1 | 4.4*1012 | 3027 |
| 8 | 1350℃-1100℃ | 1.9 | 2.4*1012 | 2440 |
| 9 | 1350℃-1100℃ | 1.5 | 3.3*1012 | 2817 |
| 10 | 1350℃-1100℃ | 1.8 | 3.6*1012 | 2530 |
TABLE 4 temperature rate of change of capacitance for anti-reduction X7R ultra-fine ceramic materials examples 1-10
Claims (8)
1. The medium material takes ultrafine porcelain material BaTiO 3 with the grain diameter of 100-200 nm as a main material, and takes 94.32-98.68 percent of the total weight of the medium material, and the anti-reduction X7R ultrafine ceramic material is prepared by adding various secondary additives, wherein the secondary additives account for 1.32-5.68 percent of the total weight of the medium material.
2. The ceramic material according to claim 1, wherein the secondary additive comprises one or more oxides of ZrO 2、BaCO3、WO3、Mn3O4 and rare earth element Y, dy, ho, er, which are respectively contained in percentage by mass of the total mass of the ceramic material ZrO2：0.1～0.4％、BaCO3：0.4～4％、WO3：0.02～0.08％、Mn3O4：0.2～0.8％、Re2O3：0.4～1.6％.
3. An anti-reduction X7R type superfine ceramic material and a preparation method thereof are characterized by comprising the following steps:
Step 1: the superfine BaTiO 3 powder with the grain diameter of 100-200 nm and one or more secondary additives of ZrO 2、BaCO3、WO3、Mn3O4 rare earth element oxides are ball-milled and mixed uniformly, and then are granulated and molded to obtain a green blank; wherein the addition amount of the secondary additive accounts for 1.32-5.68% of the mass sum of the primary crystal phase powder and the secondary additive;
Step 2: sintering; sintering the green body obtained in the step 1 for 2-4 hours at 1300-1350 ℃ in 1-2% H 2-N2 reducing atmosphere;
Step 3: reoxidation; and (3) carrying out reoxidation treatment on the sample obtained in the step (2) for 2 hours at 900-1100 ℃ under the protection of N 2 atmosphere containing O 2 to obtain the final anti-reduction X7R superfine ceramic material.
4. The method for preparing an anti-reduction X7R superfine ceramic material according to claim 3, wherein the secondary additives ZrO 2、BaCO3、WO3、Mn3O4 and rare earth oxide Re 2O3 in the step 1 are respectively in percentage by mass of the total mass of the ceramic material ZrO2：0.1～0.4％、BaCO3：0.4～4％、WO3：0.02～0.08％、Mn3O4：0.2～0.8％、Re2O3：0.4～1.6％.
5. The method for preparing an anti-reduction X7R ultrafine ceramic material according to claim 3 or 4, wherein the ball milling process in step 1 is: zirconium dioxide balls are used as ball milling media, deionized water is used as solvent, and ball milling is carried out for 3-16 hours according to the weight ratio of 1:3-5:0.5-1 of the material, balls and water.
6. The method for preparing an anti-reduction X7R ultrafine ceramic material according to claim 3 or 4, wherein the granulating process in step 2 is: the ball-milling mixture is dried and then mixed with polyvinyl alcohol aqueous solution to be granulated, and the granulating size is controlled to be 80-250 meshes.
7. The method for preparing an anti-reduction X7R ultrafine ceramic material according to claim 3 or 4, wherein the molding process in step 1 is: and (3) putting the pelleting material into a molding die, and performing dry press molding under the pressure of 10MPa to obtain a green blank.
8. The method for preparing an anti-reduction X7R ultrafine ceramic material according to claim 3 or 4, wherein the reoxidation process in step 3 is: the oxygen content in the N 2 atmosphere containing O 2 is 10-200 ppm.
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