CN113072376A - Oxidizing agent for grain boundary layer semiconductor ceramic substrate and coating method thereof - Google Patents
Oxidizing agent for grain boundary layer semiconductor ceramic substrate and coating method thereof Download PDFInfo
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- CN113072376A CN113072376A CN202110388803.9A CN202110388803A CN113072376A CN 113072376 A CN113072376 A CN 113072376A CN 202110388803 A CN202110388803 A CN 202110388803A CN 113072376 A CN113072376 A CN 113072376A
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- 239000007800 oxidant agent Substances 0.000 title claims abstract description 58
- 239000000919 ceramic Substances 0.000 title claims abstract description 55
- 239000000758 substrate Substances 0.000 title claims abstract description 51
- 238000000576 coating method Methods 0.000 title claims abstract description 34
- 239000004065 semiconductor Substances 0.000 title claims abstract description 11
- 239000010410 layer Substances 0.000 claims abstract description 51
- 230000001590 oxidative effect Effects 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000003985 ceramic capacitor Substances 0.000 claims abstract description 15
- 239000002356 single layer Substances 0.000 claims abstract description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 4
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000002002 slurry Substances 0.000 claims description 32
- 239000011248 coating agent Substances 0.000 claims description 24
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 8
- 239000003292 glue Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000011229 interlayer Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims description 2
- 238000010030 laminating Methods 0.000 claims description 2
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 2
- 238000001465 metallisation Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- -1 phosphate ester Chemical class 0.000 claims description 2
- 238000007747 plating Methods 0.000 claims description 2
- 239000002952 polymeric resin Substances 0.000 claims description 2
- 238000004528 spin coating Methods 0.000 claims description 2
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 2
- 229920003002 synthetic resin Polymers 0.000 claims description 2
- 238000010345 tape casting Methods 0.000 claims description 2
- 239000003989 dielectric material Substances 0.000 claims 1
- 238000009413 insulation Methods 0.000 abstract description 20
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 abstract description 10
- 230000008859 change Effects 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 6
- 239000003990 capacitor Substances 0.000 abstract description 4
- 238000010923 batch production Methods 0.000 abstract description 3
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000011161 development Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 17
- 229910000480 nickel oxide Inorganic materials 0.000 description 9
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910002370 SrTiO3 Inorganic materials 0.000 description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 description 2
- 229910052810 boron oxide Inorganic materials 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 238000005036 potential barrier Methods 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 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
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012858 packaging process Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
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Abstract
An oxidant for a grain boundary layer semiconductor ceramic substrate and a coating method thereof are disclosed, which comprises the following components by mass percent: bi2O3 40％～70％、Pb3O4 20％～50％、CuO 5％～20％、B2O3 10％～15％、Al2O3 5％～15％、NiO 0.1％～5％、MnO20.1 to 5 percent. The obtained ceramic substrate with crystal boundary layer has dielectric constant of 30000 +/-3000, dielectric loss of 0.3-0.8% and insulating resistance not less than 1011Omega, capacity temperature change rate less than or equal to +/-15% (-55-125 ℃), dielectric constantThe tolerance deviation is less than +/-10 percent, and the problems of low insulation resistance, large capacitance fluctuation range and the like of the capacitor prepared by the existing oxidant and the coating method thereof are solved. The main performance of the grain boundary layer single-layer ceramic capacitor is determined, the method is suitable for batch production, and the development of high-performance and miniaturized single-layer ceramic capacitors is promoted.
Description
Technical Field
The invention belongs to the field of ceramic capacitors, particularly belongs to the field of semiconductor ceramic capacitors, and further relates to an oxidant for a grain boundary layer semiconductor ceramic substrate and a coating method thereof.
Background
The grain boundary layer single-layer ceramic capacitor has the advantages of small size, large capacitance, small capacity temperature change rate (less than or equal to +/-15% @ -55-125 ℃), good frequency characteristic and the like, is widely applied to microwave hybrid integrated circuits, plays roles in blocking, filtering, coupling, decoupling, impedance matching, coplanar waveguide and the like, is suitable for a packaging process of micro-assembly lead bonding, and has larger and larger use amount in communication equipment.
SrTiO3As a key functional material for a grain boundary layer single-layer ceramic capacitor, the material is a typical perovskite type oxide, has no structural phase change above the Curie temperature, has good temperature stability and frequency characteristics, and is compatible with CCTO and TiO2Compared with high dielectric ceramics such as NiO and the like, the high dielectric ceramics have very low dielectric loss (less than or equal to 0.02) and excellent stability, and simultaneously have the same performance as BaTiO3The system does not cause fatigue and aging problems. Therefore, it is widely used for the production of ceramic substrates for high-performance grain boundary layer single-layer ceramic capacitors.
SrTiO3The preparation method of the grain boundary layer ceramic substrate mainly comprises a one-step method and a two-step method at present, wherein the one-step method is to add a semi-conducting agent and an insulating oxidant into SrTiO simultaneously3In the base material, under the conditions of proper atmosphere and temperature, the semi-conduction of ceramic material grains and the insulation of grain boundaries are simultaneously completed through one-time sintering; the two-step method is that firstly the semi-conduction of ceramic material crystal grains is realized by one-time sintering under the condition of reducing atmosphere, then the oxidant is coated on the surface of the semi-conducted ceramic substrate, and the semi-conducted ceramic substrate is sintered in an air sintering furnaceThe secondary sintering is carried out to realize the insulation of the grain boundary. The voltage-resistant characteristic of the grain boundary layer material prepared by the one-step method is poor, and the method is generally only suitable for preparing low-voltage (16V or 25V) grain boundary layer single-layer ceramic capacitor products. Therefore, at present, manufacturers at home and abroad generally adopt a two-step method to produce the grain boundary layer ceramic substrate, but under the influence of an oxidant and a coating process thereof, the domestic prepared grain boundary layer ceramic substrate mainly has the problems of low insulation resistance, poor capacitance consistency and the like. The Chinese patent CN 105276362B in 2017 provides a preparation method of an oxidant, but the insulation resistance of the prepared capacitor is less than 100G omega, the use voltage is below 50V, and meanwhile, the patent does not provide a coating process, so that the consistency of the electrical properties of the ceramic substrate for preparing the grain boundary layer cannot be evaluated.
Therefore, the selection of a proper oxidant formula and a preparation process technology, and how to uniformly coat the oxidant slurry on the surface of the semiconductive ceramic substrate to realize accurate and controllable thickness become technical problems to be solved in the field. At present, methods such as screen printing, infiltration and the like are mainly used for coating the oxidant, but the precise control of the coating thickness cannot be realized. This makes the capacitance fluctuation range of the prepared capacitor reach 20% -25%, and the insulation resistance can only reach 10%9Ω～1010Ω。
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The purpose of the invention is: the preparation method has the advantages of low cost, simple and convenient operation, easy realization of batch production and the like.
The purpose of the invention is: the method has the advantages that the coating uniformity is good, the coating thickness can be accurately controlled, the dielectric constant K of the prepared grain boundary layer ceramic substrate is 30000 +/-3000, the dielectric loss is 0.3-0.8%, and the insulation resistance is more than or equal to 1011Omega, the capacity temperature change rate (-55-125 ℃) is less than or equal to +/-15%, the allowable deviation of the dielectric constant can be controlled within +/-10%, and the problem that the insulation resistance of the conventional grain boundary layer single-layer ceramic capacitor in the market is lower (less than or equal to)1010Omega) and large capacitance fluctuation (more than or equal to 20 percent).
The purpose of the invention is: forming a compact, continuous grain boundary layer with high resistivity at the grain boundary, and changing the insulation resistance from the conventional 109Ω～1010Omega is lifted to 1011And the omega is increased by at least 1 order of magnitude, and meanwhile, the coating uniformity and the thickness of the oxidant slurry are accurately controlled, so that the capacitance fluctuation of the single-layer ceramic capacitor for preparing the grain boundary layer is increased to be within 10 percent from the current 20 to 25 percent.
Therefore, the invention provides an oxidant formula for an interfacial layer semiconductive ceramic substrate, which comprises the following components in percentage by mass: 40 to 70 percent of Bi2O320 to 50 percent of Pb3O45 to 20 percent of CuO and 10 to 15 percent of B2O35 to 15 percent of Al2O3NiO 0.1-5 wt% and MnO 0.1-5 wt%2。
The invention provides a preparation method of an oxidant slurry for an interlayer semiconductor ceramic substrate, which is characterized by comprising the following steps:
(1) according to the mass percentage, 5-20% of PVB and 80-95% of isopropanol are stirred and dissolved for 2 hours in a water bath at the temperature of 80 +/-10 ℃ to obtain a solution A;
(2) weighing oxide powder according to the oxidant component ratio, and ball-milling and mixing 100 parts of oxide powder, 100-300 parts of isopropanol and 1-5 parts of phosphate ester for 4-8 hours according to the weight part ratio to obtain a solution B;
(3) weighing the solution A according to 30-50% of the mass of the oxide powder, and adding the solution A into the solution B obtained in the step (2) for ball milling and mixing for 2-3 h.
(4) Filtering the mixture by filter cloth of 200 meshes to 350 meshes to obtain the oxidant slurry.
The medium grinding ball is made of zirconia, the diameter of the medium grinding ball is phi 3 mm-phi 8mm, and the addition amount of the medium grinding ball is 2 times-3 times of the weight of the main material oxide powder.
The PVB is B76, B79 or B98 high polymer resin.
The invention provides a coating method of an oxidant slurry for an interlayer semiconductor ceramic substrate, which comprises the following steps:
(1) preparing materials: an interface layer semiconductive ceramic substrate and oxidant slurry;
(2) setting parameters of a spin coater, wherein the rotating speed is 1: 200 r/min-600 r/min for 3 s-6 s; the rotating speed is 2: 1000 r/min-3000 r/min, 10 s-15 s.
(3) Slurry loading and sheet loading: the method comprises the following steps of (1) filling oxidant slurry into a glue containing device of a spin coater, and adsorbing a grain boundary layer semiconductive ceramic substrate on a sample table of the spin coater;
(4) glue homogenizing: starting a spin coater to carry out slurry dispensing and spin coating;
(5) drying: the drying temperature is 120 +/-10 ℃ and the drying time is 60-90 s;
(6) and (5) coating the other surface of the grain boundary layer semiconductive ceramic substrate according to the method from the step (3) to the step (5), so as to realize the coating of the oxidants on the front surface and the back surface of the grain boundary layer semiconductive ceramic substrate.
The oxidant slurry is stirred for 10-30 min by a stirrer before use and is horizontally kept stand for 10-15 min for use.
The coating thickness of the oxidant slurry is controlled by the technological parameters of the spin speed of the spin coater, the spin time, the slurry dispensing amount and the like, and can also be measured by the weight gain of the semi-conductive ceramic substrate before and after coating.
Compared with the prior art, the invention has the beneficial effects that: ensures the uniformity of the oxidant coating, provides good insulating property for the formed grain boundary layer, and the prepared grain boundary layer ceramic substrate has the dielectric constant K of 30000 +/-3000, the dielectric loss of 0.3-0.8 percent and the insulation resistance of more than or equal to 1011Omega, the capacity temperature change rate (-55-125 ℃) is less than or equal to +/-15%, the allowable deviation of the dielectric constant can be controlled within +/-10%, the oxidant and the coating method thereof are convenient for process control and realization, are suitable for batch production, determine the main performance of the grain boundary layer single-layer ceramic capacitor, and promote the development of high-performance and miniaturized single-layer ceramic capacitors.
Drawings
FIG. 1 is a graph showing the change of capacitance with temperature of the samples S1, S2, S3, S4 and S5 prepared according to the present invention.
FIG. 2 is a schematic diagram of the electrical property consistency test sampling standard of samples prepared according to the present invention.
FIG. 3 is a graph showing the capacitance uniformity of samples prepared according to the present invention.
FIG. 4 is a graph showing the insulation resistance uniformity of samples prepared according to the present invention.
Detailed Description
The first embodiment is as follows: preparation and test of grain boundary layer single-layer ceramic capacitor
(1) Preparing materials and mixing: with SrCO3、TiO2As main material, Dy2O3And Ho2O3As a donor additive, performing ball milling and mixing for 14-18 h to obtain casting slurry;
(2) tape casting and rubber discharge: casting, cutting, laminating and cutting to obtain a ceramic substrate green body, and performing glue discharging treatment at 500-700 ℃;
(3) sintering in a reducing atmosphere: the ceramic green body after rubber discharge is on N2And H2Sintering at 1200-1500 ℃ under the condition of mixed atmosphere to obtain a grain boundary layer semiconductive ceramic substrate;
(4) and (3) oxidant coating: the prepared oxidant slurry is uniformly coated on the front surface and the back surface of a semiconductive ceramic substrate by using the glue homogenizing mode provided by the invention;
(5) oxidizing and sintering: placing the semiconductive ceramic substrate coated with the oxidant on the surface in an air sintering furnace, and keeping the temperature at 950-1150 ℃ for 2-3 h to obtain a grain boundary layer insulating ceramic substrate;
(6) metallization and cutting: plating Au electrodes on the front and back surfaces of an insulating ceramic substrate of a grain boundary layer by utilizing a magnetron sputtering technology, and mechanically cutting to obtain a test sample with the size of 1mm (length) multiplied by 1mm (width) multiplied by 0.152mm (thickness);
(7) and (3) testing: an Agilent Technologies E4981A LCR tester is adopted to detect the capacitance and dielectric loss of a test sample under the conditions of the temperature of 23 ℃ plus or minus 2 ℃, the relative humidity of 40-60%, the voltage of 1V and the frequency of 1KHz plus or minus 50Hz, a dielectric temperature spectrum measuring system is adopted to test the capacitance temperature change rate of the test sample, and a homonymy TH2681 insulation resistance tester is adopted to test the insulation resistance of the test sample under the conditions of the temperature of 23 ℃ plus or minus 2 ℃, the relative humidity of 40-60%, the test voltage of 50V and the test time of 60 s. The coating thickness was examined using a Phenom Prox type scanning electron microscope.
Example two: al (Al)2O3、NiO、MnO2Influence of doping
(1) 90g of isopropanol is weighed and placed in a beaker, 10g of BP76 type PVB is weighed and stirred and dissolved in a water bath at the temperature of 80 ℃ for 2 hours to obtain a solution A.
(2) Bismuth oxide (Bi) was weighed in accordance with the oxidant ratio shown in Table 12O3) Lead tetraoxide (Pb)3O4) Copper oxide (CuO), boron oxide (B)2O3) Alumina (Al)2O3) Nickel oxide (NiO) and manganese dioxide (MnO)2) The total amount of the powder is 100g, and the purity of the raw materials is analytically pure. In addition, 300g of zirconium oxide medium grinding balls with the diameter of phi 3mm, 300g of isopropanol and 4g of phosphate are weighed and mixed by ball milling for 8 hours to obtain a solution B.
(3) And (3) weighing 50g of the solution A, adding the solution A into the solution B obtained in the step (2), carrying out ball milling and mixing for 3 hours, and filtering through 300-mesh filter cloth to obtain oxidant slurry Y1 and Y2.
(4) The same glue homogenizing parameters are adopted, the oxidant slurry Y1 and the oxidant slurry Y2 are respectively coated on the front surface and the back surface of the same batch of grain boundary layer semiconductive ceramic substrates, the grain boundary layer ceramic substrates are prepared after oxidation sintering, and the measured dielectric property results are shown in table 2 and can be obviously shown: al (Al)2O3、NiO、MnO2The doped sample has lower dielectric loss and insulation resistance of 1 multiplied by 1011Omega order of magnitude, improved by nearly 1 order of magnitude over the undoped sample.
TABLE 1 oxidizing agent ratio
Table 2 results of dielectric property test of examples two
Example three: preparation of oxidizer slurry and coating test
(1) 90g of isopropanol is weighed and placed in a beaker, 10g of BP76 type PVB is weighed and stirred and dissolved in a water bath at the temperature of 80 ℃ for 2 hours to obtain a solution A.
(2) Weighing the following raw materials, wherein bismuth oxide (Bi)2O3)31g of lead tetraoxide (Pb)3O4)38g, copper oxide (CuO)12g, boron oxide (B)2O3)8g of alumina (Al)2O3)6g, Nickel oxide (NiO)2g, manganese dioxide (MnO)2)3g, the purity of the raw materials is analytically pure. In addition, 200g of zirconium oxide medium grinding balls with the diameter of phi 5mm, 150g of isopropanol and 3g of phosphate are weighed and mixed by ball milling for 5 hours to obtain a solution B.
(3) And (3) weighing 36g of the solution A, adding the solution A into the solution B obtained in the step (2), carrying out ball milling and mixing for 2 hours, and filtering through 300-mesh filter cloth to obtain oxidant slurry.
(4) And (3) coating the oxidant slurry which is fully and uniformly stirred on the front surface and the back surface of the same batch of grain boundary layer semiconductive ceramic substrates by using a spin coater, and drying at 100 ℃ for 60s, wherein the coating parameters are shown in table 3, and the dielectric property test results are shown in table 4. FIG. 1 is the curves of the change of capacitance with temperature of the samples S1, S2, S3, S4 and S5, and it can be seen that all the tested samples show nearly linear decrease trend of capacitance with temperature increase in a wider temperature range of-55 deg.C to 150 deg.C, and have good temperature characteristics within +/-15% of the fluctuation range of the capacitance.
TABLE 3 coating parameters
Table 4 results of the three dielectric property tests of the examples
In addition, the above-mentioned coated samples were randomly sampled to prepare test samples of desired sizes, and capacitance and insulation resistance tests were performed at corresponding positions as shown in fig. 2. In FIG. 3, the capacitance distribution diagram shows that the capacitance uniformity of samples in different regions can be controlled within. + -. 10%. Fig. 4 is an insulation resistance distribution diagram, and it can be seen that the insulation resistance values of samples in different areas are relatively consistent without obvious discrete points.
As can be seen from the above examples, Al2O3、NiO、MnO2The doping of the oxides improves the compactness of a formed crystal boundary layer, reduces dielectric loss, increases the resistivity of the crystal boundary, improves the barrier of the crystal boundary and inhibits the flow of carriers on two sides of the crystal boundary. In addition, with the increase of the coating thickness of the oxidant, the dielectric constant of the ceramic substrate of the grain boundary layer is gradually reduced, and the dielectric loss and the insulation resistance are gradually increased. The dielectric constant is reduced because the thickness of the grain boundary insulating layer is increased along with the increase of the coating thickness of the oxidizing agent, namely the thickness of the effective dielectric layer is increased, and the dielectric constant is reduced along with the increase of the thickness of the grain boundary insulating layer according to the principle of a grain boundary layer capacitor. The reason why the insulation resistance gradually increases is that NiO and MnO are increased with the content of the oxidizing agent2The content of the modified additive is correspondingly increased, the grain boundary potential barrier is improved, and the grain boundary resistivity is further improved. On the other hand, the decrease of the dielectric constant leads to the decrease of the unit energy storage density, the increase of the grain boundary potential barrier and the increase of the insulation resistance. The increasing dielectric loss is mainly due to the increased content of the oxidizing agent resulting in increased defects in the grain boundaries.
Finally, it should be noted that: the above examples are merely examples for clarity of illustration, and the present invention includes but is not limited to the above examples, which are not necessarily exhaustive of all embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Embodiments that meet the requirements of the present invention are within the scope of the present invention.
Claims (10)
1. An oxidant for an interfacial layer semiconductive ceramic substrate, characterized in that the oxidant component comprises, by mass: 40 to 70 percent of Bi2O320 to 50 percent of Pb3O45 to 20 percent of CuO and 10 to 15 percent of B2O35 to 15 percent of Al2O3NiO 0.1-5 wt% and MnO 0.1-5 wt%2。
2. The oxidizing agent for an interlayer semiconductive ceramic substrate according to claim 1, wherein the purity of each component of the oxidizing agent is analytically pure or higher.
3. The method for preparing an oxidant slurry for an interlayer semiconductor ceramic substrate according to claim 1, comprising the steps of:
(1) according to the mass percentage, 5-20% of PVB and 80-95% of isopropanol are stirred and dissolved for 2 hours in a water bath at the temperature of 80 +/-10 ℃ to obtain a solution A;
(2) weighing oxide powder according to the oxidant component ratio, and ball-milling and mixing 100 parts of oxide powder, 100-300 parts of isopropanol and 1-5 parts of phosphate ester for 4-8 hours according to the weight part ratio to obtain a solution B;
(3) weighing the solution A according to 30-50% of the mass of the oxide powder, and adding the solution A into the solution B obtained in the step (2) for ball milling and mixing for 2-3 h;
(4) filtering the mixture by filter cloth of 200 meshes to 350 meshes to obtain the oxidant slurry.
4. The method for preparing an oxidant slurry for an intergranular semiconductive ceramic substrate according to claim 3, wherein the grinding ball dielectric material is zirconia and has a diameter of from 3mm to 8 mm.
5. The method for preparing an oxidant slurry for an intergranular semiconductive ceramic substrate according to claim 3, wherein the weight of the zirconia is 2 to 3 times the weight of the oxide powder.
6. The method for preparing the oxidant paste for an interlayer semiconductor ceramic substrate according to claim 3, wherein the PVB is B76, B79 or B98 polymer resin.
7. The method of coating an oxide slurry for an interlayer semiconductor ceramic substrate according to any one of claims 3 to 6, comprising the steps of:
(1) preparing materials: an interface layer semiconductive ceramic substrate and oxidant slurry;
(2) setting parameters of a spin coater, wherein the rotating speed is 1: 200 r/min-600 r/min for 3 s-6 s; the rotating speed is 2: 1000 r/min-3000 r/min for 10 s-15 s;
(3) slurry loading and sheet loading: the method comprises the following steps of (1) filling oxidant slurry into a glue containing device of a spin coater, and adsorbing a grain boundary layer semiconductive ceramic substrate on a sample table of the spin coater;
(4) glue homogenizing: starting a spin coater to carry out slurry dispensing and spin coating;
(5) drying: the drying temperature is 120 +/-10 ℃ and the drying time is 60-90 s;
(6) and (5) coating the other surface of the grain boundary layer semiconductive ceramic substrate according to the method from the step (3) to the step (5), so as to realize the coating of the oxidants on the front surface and the back surface of the grain boundary layer semiconductive ceramic substrate.
8. The method of claim 7, wherein the thickness of the oxide layer is 1 μm to 9 μm.
9. The method for coating an oxidizing agent for an interlayer semiconductor ceramic substrate according to claim 7, wherein the oxidizing agent slurry is stirred for 10 to 30min and horizontally left standing for 10 to 15min before use.
10. A preparation method of a grain boundary layer single-layer ceramic capacitor is characterized by comprising the following steps:
(1) preparing materials and mixing: with SrCO3、TiO2As main material, Dy2O3And Ho2O3As a donor additive, performing ball milling and mixing for 14-18 h to obtain casting slurry;
(2) tape casting and rubber discharge: casting, cutting into pieces, laminating and cutting to obtain a ceramic substrate green body, and performing glue discharging treatment at 500-700 ℃;
(3) sintering in a reducing atmosphere: the ceramic green body after rubber discharge is on N2And H2Sintering at 1200-1500 ℃ under the condition of mixed atmosphere to obtain a grain boundary layer semiconductive ceramic substrate;
(4) and (3) oxidant coating: uniformly coating the oxidant slurry according to any one of claims 3 to 6 on the front and back surfaces of the grain boundary layer semiconductive ceramic substrate by the coating method according to claim 7;
(5) oxidizing and sintering: placing the semiconductive ceramic substrate coated with the oxidant on the surface in an air sintering furnace, and keeping the temperature at 950-1150 ℃ for 2-3 h to obtain a grain boundary layer ceramic substrate;
(6) metallization and cutting: and plating Au electrodes on the front surface and the back surface of the ceramic substrate of the grain boundary layer by utilizing a magnetron sputtering technology, and mechanically cutting to obtain the single-layer ceramic capacitor of the grain boundary layer.
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