CN108530067A - A kind of Sm, Al codope substitution Nd1.9Sr0.1NiO4Giant dielectric ceramics and preparation method thereof - Google Patents

A kind of Sm, Al codope substitution Nd1.9Sr0.1NiO4Giant dielectric ceramics and preparation method thereof Download PDF

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CN108530067A
CN108530067A CN201710128538.4A CN201710128538A CN108530067A CN 108530067 A CN108530067 A CN 108530067A CN 201710128538 A CN201710128538 A CN 201710128538A CN 108530067 A CN108530067 A CN 108530067A
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nio
codope
powder
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CN108530067B (en
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郭旺
黄集权
江亚彬
李国京
薛锤兵
邓种华
兰海
陈剑
刘著光
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Fujian Institute of Research on the Structure of Matter of CAS
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Abstract

The invention discloses a kind of Sm, Al codopes to replace Nd1.9Sr0.1NiO4Giant dielectric ceramics and preparation method thereof.A part of Nd is replaced to replace a part of Ni with chemical general formula Nd by Al by Sm1.9‑xSmxSr0.1Ni1.0‑yAlyO4It indicates, wherein x=0.05~0.2, y=0.05~0.2.Sm, Al codope provided by the invention replaces Nd1.9Sr0.1NiO4Giant dielectric ceramic material is effectively improved the dielectric properties of product, and preparation method is simply and reproducible, and does not need additional atmosphere assisted sintering.

Description

A kind of Sm, Al codope substitution Nd1.9Sr0.1NiO4Giant dielectric ceramics and preparation method thereof
Technical field
The invention belongs to dielectric ceramic material technical fields, and in particular to a kind of Sm, Al codope substitution Nd1.9Sr0.1NiO4Giant dielectric ceramics and preparation method thereof.
Background technology
With the fast development of microelectronic industry, the electronic components such as ceramic capacitor gradually towards micromation, it is integrated, Intelligent direction develops.To improve the storage density of memory, it is ensured that signal can be stored on smaller area, it is necessary to Using the lower dielectric substance of dielectric constant lossy come ensure reduce dielectric substance size simultaneously, do not influence capacitance Amount and leakage current.Therefore the research of the dielectric substance of high-k, low-dielectric loss has been to be concerned by more and more people.
Nd2-xSrxNiO4Ceramics belong to K2NiF4The nickelate structural ceramics of structure, wherein Nd1.5Sr0.5NiO4Ceramics Dielectric constant is higher in room temperature, but its excessively high dielectric loss make it difficult to apply it is normal in the high dielectric such as capacitor, reservoir In several electronic components.Application No. is a kind of zirconium doping vario-property is disclosed in 201310188414.7 Chinese patent La2NiMnO6Ceramic dielectric material with adjustable and preparation method thereof.The preparation method can be improved by using zirconium doping vario-property La2NiMnO6The dielectric constant of ceramics.However, modified La2NiMnO6The dielectric loss of ceramic dielectric material with adjustable is but up to 14.45, prevent it from the use demand that meets electronics industry.
Invention content
Based on the above issues, the purpose of the present invention is to provide a kind of Sm, Al codopes to replace Nd1.9Sr0.1NiO4Huge Jie Electroceramics and preparation method thereof.
The technical solution adopted in the present invention is to solve above-mentioned technical problem：
A kind of Sm, Al codope substitution Nd1.9Sr0.1NiO4Giant dielectric ceramics, replace a part of Nd by Sm, replace one by Al Part Ni, chemical formula Nd1.9-xSmxSr0.1Ni1.0-yAlyO4, wherein x=0.05~0.20, y=0.05~0.20.
Preferably x=0.08~0.12, y=0.08~0.12.
It is further preferred that x=0.09~0.11, y=0.09~0.11.For example, x=0.10, y=0.10.
Wherein, Sm, Al codope replaces Nd1.9Sr0.1NiO4The principal crystalline phase of giant dielectric ceramics is K2NiF4The nickel of structure Hydrochlorate structure.
Wherein, Sm, Al codope replaces Nd1.9Sr0.1NiO4The ceramic crystalline grain of giant dielectric ceramics is 5 μm.
The present invention also provides Sm, Al codopes as described above to replace Nd1.9Sr0.1NiO4The preparation method of giant dielectric ceramics, Include the following steps：
(1) by Nd1.9Sr0.1NiO4Powder, Sm2O3And Al2O3Ball milling mixing after addition dispersant, composite powder is obtained after drying Body；
(2) it is granulated and is sieved after composite granule being added binder, be molded, then dumping obtains ceramic body；
(3) by ceramic body through oversintering, up to product after furnace cooling cooling.
In step (1), the raw material Nd1.9Sr0.1NiO4Powder, Sm2O3And Al2O3Nd is obtained according to stoichiometric ratio1.9- xSmxSr0.1Ni1.0-yAlyO4, wherein x=0.05~0.20, y=0.05~0.20.Such as raw material Nd1.9Sr0.1NiO4Powder, Sm2O3And Al2O3Molar ratio be 1：1：1.
In step (1), the dispersant is ethyl alcohol, preferably absolute ethyl alcohol.
In step (1), the raw material：Ball：The mass ratio of dispersant is (1-2)：(9-12)：(5-10), preferably 1：10： 5。
In step (1), the time of the ball milling is 10-16 hours, and as illustrative example, Ball-milling Time is 16 small When.
In step (2), the binder is the polyvinyl alcohol water solution of 1-5wt%, the polyvinyl alcohol water of preferably 5wt% Solution.
In step (2), the dosage of the binder is the 5-15wt% of the composite granule weight obtained in step (1).
In step (2), the step of granulation, is：Composite granule is taken, is ground after binder is added.
Preferably, the milling time is 0.2-1.5 hours, preferably 0.5-1 hours；
In step (2), it is described sieving be 100-120 mesh sieve, preferably 120 mesh sieve.
In step (2), described molding steps are as follows：Composite granule after sieving is pressed into disk, through isostatic cool pressing It obtains.
In step (2), described be molded under the pressure of 15-20MPa is suppressed.
In step (2), the step of the molding in the diameter of disk can be 9-12mm, preferably 10mm；
In step (2), the thickness of the disk can be 1-2mm, preferably 1.5mm.
In step (2), the step of the molding in, the pressure of isostatic cool pressing process is 180-200MPa, preferably 190MPa；
In step (2), the dwell time of the isostatic cool pressing process is 1-3min, preferably 2min.
In step (2), kept the temperature afterwards for disk after molding is placed in Muffle furnace first to heat up the step of the dumping, finally Cooled to room temperature.
In step (2), the rate of the heating can be 1-3 DEG C/min, preferably 1 DEG C/min；
In step (2), the temperature of the heating can be 500-650 DEG C, preferably 600 DEG C；
In step (2), the time of the heat preservation is 90-150min, preferably 120-140min.
In step (3), the sintering temperature can be 1200-1400 DEG C, preferably 1300-1350 DEG C, for example, 1330 ℃。
In step (3), the sintering time is 1-6h, can be 3h as illustrative example.
The present invention also provides the Nd1.9Sr0.1NiO4Raw powder's production technology includes the following steps：
(a) by raw material Nd2O3, NiO and SrCO3Absolute ethyl alcohol ball milling is added, pre-burning powder is obtained after drying sieving；
(b) it after keeping the temperature the pre-burning powder obtained in step (a), is obtained after secondary ball milling, drying and screening Nd1.9Sr0.1NiO4Powder.
In step (a), raw material Nd2O3, NiO and SrCO3Molar ratio be 0.95：1：0.1.
In step (a), the raw material：Ball：The mass ratio of absolute ethyl alcohol is 1：10：5.
In step (a), the Ball-milling Time is 8-10h, for example, 10h.
In step (a), the sieving was 100-120 mesh sieve；Preferably cross 120 mesh sieve.
In step (b), the holding temperature is 900-1200 DEG C；Preferably 1050-1100 DEG C, for example, 1100 DEG C.
In step (b), the soaking time is 1-3h, is 3h as illustrative example.
In step (b), the time of the ball milling is 8-10h, for example, 10h.
In step (b), the sieving was 100-120 mesh sieve, was preferably sieved with 100 mesh sieve.
Compared with prior art, the beneficial effects of the present invention are：
1) present invention is by Nd1.9Sr0.1NiO4Different location micro ion substitution is carried out, Ni is replaced by Al, is taken by Sm Make to form very strong interfacial polarization inside ceramics for Nd, generate giant dielectric phenomenon, while donor doping and acceptor doping is mutual Under effect, the movement of electronics is limited to a certain extent, and the height for reducing individually incorporation different ions and generating is lost, and obtains The Nd of huge dielectric constant1.9-xSmxSr0.1Ni1.0-yAlyO4Ceramic material (frequency range of 1000-10MHz).
2) Sm, Al codope substitution Nd that the present invention is prepared1.9Sr0.1NiO4Giant dielectric ceramic material with Nd1.9Sr0.1NiO4Ceramic phase ratio, the dielectric constant at room temperature (25 DEG C) 2KHz are increased to 560241 by 26904, dielectric loss It is reduced to 0.987 by 34.684.
3) Sm, Al codope of the invention replaces Nd1.9Sr0.1NiO4The principal crystalline phase of giant dielectric ceramics is K2NiF4Structure Nickelate structure, the fine and close distribution of ceramic crystalline grain, and there is not dephasign.
4) Sm, Al codope substitution Nd that the present invention is prepared1.9Sr0.1NiO4Giant dielectric ceramic material is in very wide frequency Huge dielectric constant is kept within the scope of rate, preparation method is simple for process, short preparation period, does not need additional atmosphere auxiliary and burns Knot, it is easily operated, it can be achieved that industrialized production.
Description of the drawings
Fig. 1 is comparative example 1Nd1.9Sr0.1NiO4Ceramics and embodiment 2Nd1.8Sm0.1Sr0.1Ni0.9Al0.1O4The X of ceramics sample X ray diffration pattern x.
Fig. 2 is comparative example 1Nd1.9Sr0.1NiO4Ceramics and embodiment 2Nd1.8Sm0.1Sr0.1Ni0.9Al0.1O4Ceramics sample exists The relation curve of dielectric constant and frequency at room temperature.
Fig. 3 is comparative example 1Nd1.9Sr0.1NiO4Ceramics and embodiment 2Nd1.8Sm0.1Sr0.1Ni0.9Al0.1O4Ceramics sample exists The relation curve of dielectric loss and frequency at room temperature.
Fig. 4 is comparative example 1Nd1.9Sr0.1NiO4The scanning electron microscope (SEM) photograph of ceramics.
Fig. 5 is embodiment 2Nd1.8Sm0.1Sr0.1Ni0.9Al0.1O4The scanning electron microscope (SEM) photograph of ceramics sample.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention Rather than it limits the scope of the invention.Furthermore, it is to be understood that after having read recorded content of the invention, this field skill Art personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within limited range of the present invention.
Unless otherwise indicated, the raw materials and reagents used in embodiment are commercial materials.
Embodiment 1Nd1.9Sr0.1NiO4The preparation of powder
1) raw material 6.3931gNd is taken2O3, 1.4938gNiO and 0.2953gSrCO3, using absolute ethyl alcohol as dispersant, by matter Amount compares raw material：Ball：Absolute ethyl alcohol=1：10：5, ball milling 10 hours obtained pre-burning powder after drying 120 mesh sieve；
2) after the pre-burning powder for obtaining step 1) keeps the temperature 3h at 1100 DEG C, through secondary ball milling 10 hours, dried 100 mesh Nd is obtained after sieve1.9Sr0.1NiO4Powder.
Comparative example 1Nd1.9Sr0.1NiO4The preparation of ceramics
1) by Nd1.9Sr0.1NiO4The polyvinyl alcohol water solution that 5wt% is added in powder is granulated and is sieved, and weighs 2g's Granulation powder will add the pressed by powder of binder into the circle of diameter 10mm, thickness about 1.5mm under the pressure of 15-20MPa Piece obtains ceramic body using the isostatic cool pressing in 200MPa pressurizes 2min.
2) ceramic body after molding is needed to exclude polyvinyl alcohol colloid before sintering, the actual temp system of dumping is such as Under：600 DEG C are risen to according to the heating rate of 1 DEG C/min and keep the temperature 120min, cooled to room temperature in Muffle furnace.
3) ceramic body after dumping, which is placed in high temperature furnace, is sintered, and does not need special atmosphere assisted sintering.Sintering Actual temp system is：900 DEG C first are warming up to the heating rate of 3 DEG C/min, is then warming up to the heating rate of 2 DEG C/min 1330 DEG C and keep the temperature 3 hours, later with stove natural cooling cool down.
Embodiment 2Nd1.8Sm0.1Sr0.1Ni0.9Al0.1O4The preparation of ceramics sample
1) by raw material 6.0758gNd1.9Sr0.1NiO4、5.2308gSm2O3And 1.5294gAl2O3, it is dispersion with absolute ethyl alcohol Agent, in mass ratio mixture：Ball：Absolute ethyl alcohol=1：10：5, ball milling mixing 16 hours after absolute ethyl alcohol is added, is obtained after drying Nd1.8Sm0.1Sr0.1Ni0.9Al0.1O4Powder；
2) 1.2g composite granules are added to the polyvinyl alcohol water solution of 0.5m l5wt%, grinds 0.5 hour and makes in mortar Grain crosses 120 mesh mesh screens, the disk of diameter 10mm, thickness about 1.5mm is then pressed at 15MPa, using at 200MPa The isostatic cool pressing of pressurize 2min obtains ceramic body.Ceramic body is finally subjected to dumping operation.The step of dumping is will be ceramic Green body, which is placed in Muffle furnace, to be risen to 600 DEG C according to the heating rate of 1 DEG C/min and keeps the temperature 120min, cooled to room temperature；
3) ceramic body that step 2) obtains is sintered 3 hours at 1330 DEG C and obtains Nd1.8Sm0.1Sr0.1Ni0.9Al0.1O4 Ceramics sample.
Comparative example 1 of the present invention, 2 sample of embodiment are subjected to XRD characterization, the results are shown in Figure 1 by the XRD of sample.It can by Fig. 1 To find out, the Nd of sintering1.8Sm0.1Sr0.1Ni0.9Al0.1O4The principal crystalline phase of ceramics sample is K2NiF4The nickelate structure of structure is made pottery There is not dephasign in porcelain, illustrates that Sm and Al have completely passed into Nd1.9Sr0.1NiO4In crystal.
Embodiment 2, the dielectric and magnetic figure of 1 sample of comparative example are as shown in Figure 2 and Figure 3.Fig. 2 corresponding is dielectric constant and frequency The relational graph of rate；It is the relational graph of dielectric loss and frequency that Fig. 3 is corresponding.It can be seen from Fig. 2 and Fig. 3 Nd1.8Sm0.1Sr0.1Ni0.9Al0.1O4Dielectric constant relative to Nd1.9Sr0.1NiO4(maximum dielectric constant is by 26114 for increase It increases to 60524), and minimum dielectric loss is reduced to 0.1162 by 0.1847.
Comparative example 1, the scanning electron microscope collection of illustrative plates of 2 sample of embodiment are as shown in Figure 4, Figure 5.Embodiment 2 as seen from Figure 4 The fine and close distribution of ceramic crystalline grain, and after the substitution of Sm, Al codope, ceramic crystalline grain increases to 5 μm or so by 2 μm.
More than, embodiments of the present invention are illustrated.But the present invention is not limited to the above embodiments.It is all Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the guarantor of the present invention Within the scope of shield.

Claims (10)

1. a kind of Sm, Al codope replaces Nd1.9Sr0.1NiO4Giant dielectric ceramics, which is characterized in that a part of Nd is replaced by Sm, by Al replaces a part of Ni, chemical formula Nd1.9-xSmxSr0.1Ni1.0-yAlyO4, wherein x=0.05~0.2, y=0.05~ 0.2。
2. Sm, Al codope as described in claim 1 replaces Nd1.9Sr0.1NiO4Giant dielectric ceramics, which is characterized in that x=0.08 ~0.12, y=0.08~0.12.
Preferably, x=0.09~0.11, y=0.09~0.11.For example, x=0.10, y=0.10.
3. Sm, Al codope as claimed in claim 1 or 2 replaces Nd1.9Sr0.1NiO4Giant dielectric ceramics, which is characterized in that it is led Crystalline phase is K2NiF4The nickelate structure of structure.
Preferably, ceramic crystalline grain is 5 μm.
4. Sm, Al codope replace Nd as described in claim any one of 1-31.9Sr0.1NiO4The preparation method of giant dielectric ceramics, It is characterised in that it includes following steps：
(1) by Nd1.9Sr0.1NiO4Powder, Sm2O3And Al2O3Ball milling mixing after addition dispersant, composite granule is obtained after drying；
(2) it is granulated and is sieved after composite granule being added binder, be molded, then dumping obtains ceramic body；
(3) by ceramic body through oversintering, up to product after furnace cooling cooling.
5. Sm, Al codope as claimed in claim 4 replaces Nd1.9Sr0.1NiO4The preparation method of giant dielectric ceramics, feature exist In, in step (1), the raw material Nd1.9Sr0.1NiO4Powder, Sm2O3And Al2O3Nd is obtained according to stoichiometric ratio1.9- xSmxSr0.1Ni1.0-yAlyO4, wherein x=0.05~0.20, y=0.05~0.20.Such as raw material Nd1.9Sr0.1NiO4Powder, Sm2O3And Al2O3Molar ratio be 1：1：1.
In step (1), it is preferable that the dispersant is ethyl alcohol, further preferably absolute ethyl alcohol.
In step (1), it is preferable that the raw material：Ball：The mass ratio of dispersant is (1-2)：(9-12)：(5-10), it is further excellent It is selected as 1：10：5.
In step (1), it is preferable that the time of the ball milling is 10-16 hours, such as Ball-milling Time is 16 hours.
6. Sm, Al codope replace Nd as described in claim 4 or 51.9Sr0.1NiO4The preparation method of giant dielectric ceramics, feature It is, in step (2), the binder is the polyvinyl alcohol water solution of 1-5wt%, and the preferably polyvinyl alcohol of 5wt% is water-soluble Liquid.
In step (2), it is preferable that the dosage of the binder is the 5-15wt% of the composite granule weight obtained in step (1).
In step (2), it is preferable that the step of granulation is：Composite granule is taken, is ground after binder is added,
In step (2), it is preferable that the milling time is 0.2-1.5 hours, further preferably 0.5-1 hours；
In step (2), it is preferable that it is described sieving be 100-120 mesh sieve, further preferably 120 mesh sieve.
In step (2), it is preferable that described molding steps are as follows：Composite granule after sieving is pressed into disk, through cold etc. quiet Pressure obtains.
In step (2), it is preferable that described be molded under the pressure of 15-20MPa is suppressed.
In step (2), it is preferable that the diameter of disk can be 9-12mm, preferably 10mm in the step of the molding；
In step (2), it is preferable that the thickness of the disk can be 1-2mm, further preferably 1.5mm.
In step (2), it is preferable that in the step of the molding, the pressure of isostatic cool pressing process is 180-200MPa, preferably 190MPa；
In step (2), it is preferable that the dwell time of the isostatic cool pressing process is 1-3min, further preferably 2min.
In step (2), it is preferable that it is kept the temperature afterwards for disk after molding is placed in Muffle furnace first to heat up the step of the dumping, Last cooled to room temperature.
In step (2), it is preferable that the rate of the heating can be 1-3 DEG C/min, further preferably 1 DEG C/min；
In step (2), it is preferable that the temperature of the heating can be 500-650 DEG C, further preferably 600 DEG C；
In step (2), it is preferable that the time of the heat preservation is 90-150min, further preferably 120-140min.
7. Sm, Al codope replace Nd as described in claim any one of 4-61.9Sr0.1NiO4The preparation method of giant dielectric ceramics, It is characterized in that, in step (3), the sintering temperature can be 1200-1400 DEG C, preferably 1300-1350 DEG C, for example, 1330℃。
In step (3), it is preferable that the sintering time is 1-6h, such as can be 3h.
8. a kind of Nd1.9Sr0.1NiO4Raw powder's production technology, which is characterized in that include the following steps：
(a) by raw material Nd2O3, NiO and SrCO3Absolute ethyl alcohol ball milling is added, pre-burning powder is obtained after drying sieving；
(b) after keeping the temperature the pre-burning powder obtained in step (a), Nd is obtained after secondary ball milling, drying and screening1.9Sr0.1NiO4Powder Body.
9. Nd as claimed in claim 81.9Sr0.1NiO4Raw powder's production technology, which is characterized in that in step (a), raw material Nd2O3, NiO and SrCO3Molar ratio be 0.95：1：0.1.
In step (a), it is preferable that the raw material：Ball：The mass ratio of absolute ethyl alcohol is 1：10：5.
In step (a), it is preferable that the Ball-milling Time is 8-10h, for example, 10h.
In step (a), it is preferable that the sieving was 100-120 mesh sieve；Further preferably cross 120 mesh sieve.
10. the Nd as described in claim 8 or 91.9Sr0.1NiO4Raw powder's production technology, which is characterized in that described in step (b) Holding temperature is 900-1200 DEG C；Preferably 1050-1100 DEG C, for example, 1100 DEG C.
In step (b), it is preferable that the soaking time is 1-3h, is such as 3h.
In step (b), it is preferable that the time of the ball milling is 8-10h, for example, 10h.
In step (b), it is preferable that the sieving was 100-120 mesh sieve, was further preferably sieved with 100 mesh sieve.
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