CN101747030A - Magneto-electricity composite material with huge dielectric constant and high magnetic conductivity and preparation method thereof - Google Patents

Magneto-electricity composite material with huge dielectric constant and high magnetic conductivity and preparation method thereof Download PDF

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CN101747030A
CN101747030A CN200910254522A CN200910254522A CN101747030A CN 101747030 A CN101747030 A CN 101747030A CN 200910254522 A CN200910254522 A CN 200910254522A CN 200910254522 A CN200910254522 A CN 200910254522A CN 101747030 A CN101747030 A CN 101747030A
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杨海波
林营
王芬
朱建锋
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Shaanxi University of Science and Technology
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Abstract

具有巨介电常数和高磁导率的磁电复合材料及其制备方法，首先，按xNi0.8Zn0.2Fe2O4/(1-x)Ba0.6Sr0.4TiO3的体积比将Ni0.8Zn0.2Fe2O4和Ba0.6Sr0.4TiO3粉体混合均匀得混合料，其中0.6≤x≤0.9；其次，加入PVA粘合剂造粒，经60目与120目筛网过筛，得到所需复合材料的混合粉末；最后，将复合材料的混合粉末按需要压制成型，在550℃，保温4小时，再在1300～1350℃下烧结0.5～2小时成瓷，即得到具有巨介电常数和高磁导率的磁电复合材料的。所述的具有巨介电常数和高磁导率的磁电复合材料在100Hz下介电常数为63000～156000，在10MHz下磁导率为5.3～29。Magnetoelectric composite material with giant permittivity and high magnetic permeability and its preparation method , firstly, Ni 0.8 Zn 0.2 Fe 2 O 4 and Ba 0.6 Sr 0.4 TiO 3 powders were evenly mixed to obtain a mixture, wherein 0.6≤x≤0.9; secondly, adding PVA binder to granulate, and sieving through 60 mesh and 120 mesh sieves to obtain the The mixed powder of the composite material is needed; finally, the mixed powder of the composite material is pressed and molded as required, kept at 550°C for 4 hours, and then sintered at 1300-1350°C for 0.5-2 hours to form porcelain, that is, a ceramic with a large dielectric constant is obtained. and magnetoelectric composites with high permeability. The dielectric constant of the magnetoelectric composite material with giant dielectric constant and high magnetic permeability is 63,000-156,000 at 100 Hz, and the magnetic permeability is 5.3-29 at 10 MHz.

Description

Has magnetic electric compound material of huge dielectric constant and high magnetic permeability and preparation method thereof
Technical field
The invention belongs to material science, relate to a kind of magnetic electric compound material and preparation method thereof with huge dielectric constant and high magnetic permeability.
Background technology
Along with electronic industry is more and more higher for the requirement of integrated level, often on very little chip integrated components and parts number in necessarily.Therefore comprise that the microminiaturization and the miniaturization of the components and parts of electrical condenser are inexorable trends.And the big more material of effective dielectric constant takies identical resource and can obtain bigger electric capacity, thereby satisfies the function on the various circuit.Therefore, the huge dielectric constant material just can use less resources, takies volume still less.Therefore, research and develop out huge dielectric constant material efficiently and crucial meaning is arranged for the development of large-scale integrated circuit technology.In addition, along with the develop rapidly of information and radio communication technology, the size of electron device is more and more littler, and integrated level is more and more higher.This just requires electronic material to have multi-functional characteristic, for example, and magnetic dielectric properties, magneto-optical property etc.In order to satisfy the requirement of multi-functional components and parts, people just prepare the magnetic electric compound material aspect and have carried out many research work.These matrix materials have electric capacity and inductance characteristic simultaneously, can be used to prepare compact filter, antenna, EMI suppressor etc.The CaCu that has the material of huge dielectric constant at present 3Ti 4O 12Though but do not have magnetic Deng having high-k.Still there is not at present a kind of magnetic electric compound material that had both had huge dielectric constant and high magnetic permeability.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology simply to have magnetic electric compound material of huge dielectric constant and high magnetic permeability and preparation method thereof.
For achieving the above object, the preparation method that the present invention adopts is:
1) preparation Ni 0.8Zn 0.2Fe 2O 4Powder: press chemical general formula Ni 0.8Zn 0.2Fe 2O 4, take by weighing analytically pure NiO, ZnO and Fe 2O 3Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting 1170 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves with gained bulk sample pulverizing back and is obtained Ni 0.8Zn 0.2Fe 2O 4Powder;
2) preparation Ba 0.6Sr 0.4TiO 3Powder: press chemical general formula Ba 0.6Sr 0.4TiO 3, take by weighing analytically pure BaCO 3, SrCO 3And TiO 2Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1150 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Ba 0.6Sr 0.4TiO 3Powder;
3) press xNi 0.8Zn 0.2Fe 2O 4/ (1-x) Ba 0.6Sr 0.4TiO 3Volume ratio with Ni 0.8Zn 0.2Fe 2O 4And Ba 0.6Sr 0.4TiO 3Powder mix compound, 0.6≤x≤0.9 wherein;
4) the PVA tackiness agent granulation of adding mixture quality umber 8%～15% is sieved through 60 orders and 120 eye mesh screens, obtains the mixed powder of required matrix material; Described PVA tackiness agent employing mass concentration is 5% polyvinyl alcohol water solution;
5) last, with the mixed powder compression moulding on demand of matrix material,, be incubated 4 hours and get rid of tackiness agent PVA at 550 ℃, again at 0.5～2 hour one-tenth of 1300～1350 ℃ of following sintering porcelain, promptly obtain having the magnetic electric compound material of huge dielectric constant and high magnetic permeability.
Zhi Bei described composition expression formula with magnetic electric compound material of huge dielectric constant and high magnetic permeability is according to the method described above: xNi 0.8Zn 0.2Fe 2O 4/ (1-x) Ba 0.6Sr 0.4TiO 3, wherein x is Ni 0.8Zn 0.2Fe 2O 4Percent by volume, and 0.6≤x≤0.9, this matrix material specific inductivity under 100Hz is 63000～156000, magnetic permeability is 5.3～29 under 10MHz.
Description of drawings
Fig. 1 is for working as Ni 0.8Zn 0.2Fe 2O 4Volume ratio be 60%, Ba 0.6Sr 0.4TiO 3Volume ratio be the dielectric properties of 40% o'clock matrix material;
Fig. 2 is for working as Ni 0.8Zn 0.2Fe 2O 4Volume ratio be 70%, Ba 0.6Sr 0.4TiO 3Volume ratio be the dielectric properties of 30% o'clock matrix material;
Fig. 3 is for working as Ni 0.8Zn 0.2Fe 2O 4Volume ratio be 80%, Ba 0.6Sr 0.4TiO 3Volume ratio be the dielectric properties of 20% o'clock matrix material;
Fig. 4 is for working as Ni 0.8Zn 0.2Fe 2O 4Volume ratio be 90%, Ba 0.6Sr 0.4TiO 3Volume ratio be the dielectric properties of 10% o'clock matrix material;
Fig. 5 is for working as Ni 0.8Zn 0.2Fe 2O 4Volume ratio be 60%, Ba 0.6Sr 0.4TiO 3Volume ratio be the magnetic property of 40% o'clock matrix material;
Fig. 6 is for working as Ni 0.8Zn 0.2Fe 2O 4Volume ratio be 70%, Ba 0.6Sr 0.4TiO 3Volume ratio be the magnetic property of 30% o'clock matrix material;
Fig. 7 is for working as Ni 0.8Zn 0.2Fe 2O 4Volume ratio be 80%, Ba 0.6Sr 0.4TiO 3Volume ratio be the magnetic property of 20% o'clock matrix material;
Fig. 8 is for working as Ni 0.8Zn 0.2Fe 2O 4Volume ratio be 90%, Ba 0.6Sr 0.4TiO 3Volume ratio be the magnetic property of 10% o'clock matrix material.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
Embodiment 1: preparation Ni 0.8Zn 0.2Fe 2O 4Powder: press chemical general formula Ni 0.8Zn 0.2Fe 2O 4, take by weighing analytically pure NiO, ZnO and Fe 2O 3Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting 1170 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves with gained bulk sample pulverizing back and is obtained Ni 0.8Zn 0.2Fe 2O 4Powder; Preparation Ba 0.6Sr 0.4TiO 3Powder: press chemical general formula Ba 0.6Sr 0.4TiO 3, take by weighing analytically pure BaCO 3, SrCO 3And TiO 2Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1150 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Ba 0.6Sr 0.4TiO 3Powder; Press 0.6Ni again 0.8Zn 0.2Fe 2O 4/ 0.4Ba 0.6Sr 0.4TiO 3Volume percent with Ni 0.8Zn 0.2Fe 2O 4And Ba 0.6Sr 0.4TiO 3Powder mix compound; Secondly, add the PVA tackiness agent granulation of mixture quality umber 15%, sieve, obtain the mixed powder of required matrix material through 60 orders and 120 eye mesh screens; Described PVA tackiness agent employing mass concentration is 5% polyvinyl alcohol water solution; At last,,, be incubated 4 hours and get rid of tackiness agent PVA, became porcelain in 2 hours at 1350 ℃ of following sintering again, promptly obtain having the magnetic electric compound material of huge dielectric constant and high magnetic permeability at 550 ℃ with the mixed powder compression moulding on demand of matrix material.The dielectric properties of this matrix material are seen Fig. 1, and magnetic property is seen Fig. 5.
Embodiment 2: preparation Ni 0.8Zn 0.2Fe 2O 4Powder: press chemical general formula Ni 0.8Zn 0.2Fe 2O 4, take by weighing analytically pure NiO, ZnO and Fe 2O 3Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting 1170 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves with gained bulk sample pulverizing back and is obtained Ni 0.8Zn 0.2Fe 2O 4Powder; Preparation Ba 0.6Sr 0.4TiO 3Powder: press chemical general formula Ba 0.6Sr 0.4TiO 3, take by weighing analytically pure BaCO 3, SrCO 3And TiO 2Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1150 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Ba 0.6Sr 0.4TiO 3Powder; Press 0.7Ni 0.8Zn 0.2Fe 2O 4/ 0.3Ba 0.6Sr 0.4TiO 3Volume percent with Ni 0.8Zn 0.2Fe 2O 4And Ba 0.6Sr 0.4TiO 3Powder mix compound; Secondly, add the PVA tackiness agent granulation of mixture quality umber 12%, sieve, obtain the mixed powder of required matrix material through 60 orders and 120 eye mesh screens; Described PVA tackiness agent employing mass concentration is 5% polyvinyl alcohol water solution; At last,,, be incubated 4 hours and get rid of tackiness agent PVA, became porcelain in 1.5 hours at 1320 ℃ of following sintering again, promptly obtain having the magnetic electric compound material of huge dielectric constant and high magnetic permeability at 550 ℃ with the mixed powder compression moulding on demand of matrix material.The dielectric properties of this matrix material are seen Fig. 2, and magnetic property is seen Fig. 6.
Embodiment 3: preparation Ni 0.8Zn 0.2Fe 2O 4Powder: press chemical general formula Ni 0.8Zn 0.2Fe 2O 4, take by weighing analytically pure NiO, ZnO and Fe 2O 3Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting 1170 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves with gained bulk sample pulverizing back and is obtained Ni 0.8Zn 0.2Fe 2O 4Powder; Preparation Ba 0.6Sr 0.4TiO 3Powder: press chemical general formula Ba 0.6Sr 0.4TiO 3, take by weighing analytically pure BaCO 3, SrCO 3And TiO 2Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1150 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Ba 0.6Sr 0.4TiO 3Powder; Press 0.8Ni 0.8Zn 0.2Fe 2O 4/ 0.2Ba 0.6Sr 0.4TiO 3Volume percent with Ni 0.8Zn 0.2Fe 2O 4And Ba 0.6Sr 0.4TiO 3Powder mix compound; Secondly, add the PVA tackiness agent granulation of mixture quality umber 8%, sieve, obtain the mixed powder of required matrix material through 60 orders and 120 eye mesh screens; Described PVA tackiness agent employing mass concentration is 5% polyvinyl alcohol water solution; At last,,, be incubated 4 hours and get rid of tackiness agent PVA, became porcelain in 1 hour at 1310 ℃ of following sintering again, promptly obtain having the magnetic electric compound material of huge dielectric constant and high magnetic permeability at 550 ℃ with the mixed powder compression moulding on demand of matrix material.The dielectric properties of this matrix material are seen Fig. 3, and magnetic property is seen Fig. 7.
Embodiment 4: preparation Ni 0.8Zn 0.2Fe 2O 4Powder: press chemical general formula Ni 0.8Zn 0.2Fe 2O 4, take by weighing analytically pure NiO, ZnO and Fe 2O 3Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting 1170 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves with gained bulk sample pulverizing back and is obtained Ni 0.8Zn 0.2Fe 2O 4Powder; Preparation Ba 0.6Sr 0.4TiO 3Powder: press chemical general formula Ba 0.6Sr 0.4TiO 3, take by weighing analytically pure BaCO 3, SrCO 3And TiO 2Preparation back ball milling 4 hours, oven dry is sieved then, and briquetting through 1150 ℃ of pre-burnings 3 hours, is crossed 120 mesh sieves after then the gained bulk sample being pulverized and is obtained Ba 0.6Sr 0.4TiO 3Powder; Press 0.9Ni 0.8Zn 0.2Fe 2O 4/ 0.1Ba 0.6Sr 0.4TiO 3Volume percent with Ni 0.8Zn 0.2Fe 2O 4And Ba 0.6Sr 0.4TiO 3Powder mix compound; Secondly, add the PVA tackiness agent granulation of mixture quality umber 10%, sieve, obtain the mixed powder of required matrix material through 60 orders and 120 eye mesh screens; Described PVA tackiness agent employing mass concentration is 5% polyvinyl alcohol water solution; At last,,, be incubated 4 hours and get rid of tackiness agent PVA, became porcelain in 0.5 hour at 1300 ℃ of following sintering again, promptly obtain having the magnetic electric compound material of huge dielectric constant and high magnetic permeability at 550 ℃ with the mixed powder compression moulding on demand of matrix material.The dielectric properties of this matrix material are seen Fig. 4, and magnetic property is seen Fig. 8.

Claims (2)

1.具有巨介电常数和高磁导率的磁电复合材料的制备方法，其特征在于：1. have the preparation method of the magnetoelectric composite material of giant permittivity and high magnetic permeability, it is characterized in that: 1)制备Ni0.8Zn0.2Fe2O4粉体：按化学通式Ni0.8Zn0.2Fe2O4，称取分析纯的NiO，ZnO和Fe2O3配制后球磨4小时，然后烘干，过筛，压块，在1170℃预烧3小时，将所得块状样品粉碎后过120目筛得到Ni0.8Zn0.2Fe2O4粉体；1) Preparation of Ni 0.8 Zn 0.2 Fe 2 O 4 powder: according to the general chemical formula Ni 0.8 Zn 0.2 Fe 2 O 4 , weigh analytically pure NiO, ZnO and Fe 2 O 3 to prepare, ball mill for 4 hours, and then dry, Sieve, briquette, and pre-sinter at 1170°C for 3 hours, crush the resulting block sample and pass through a 120-mesh sieve to obtain Ni 0.8 Zn 0.2 Fe 2 O 4 powder; 2)制备Ba0.6Sr0.4TiO3粉体：按化学通式Ba0.6Sr0.4TiO3，称取分析纯的BaCO3，SrCO3和TiO2配制后球磨4小时，然后烘干，过筛，压块，经1150℃预烧3小时，然后将所得块状样品粉碎后过120目筛得到Ba0.6Sr0.4TiO3粉体；2) Preparation of Ba 0.6 Sr 0.4 TiO 3 powder: According to the general chemical formula Ba 0.6 Sr 0.4 TiO 3 , weigh analytically pure BaCO 3 , SrCO 3 and TiO 2 for preparation, ball mill for 4 hours, then dry, sieve, press Block, pre-calcined at 1150°C for 3 hours, then crush the obtained block sample and pass it through a 120-mesh sieve to obtain Ba 0.6 Sr 0.4 TiO 3 powder; 3)按xNi0.8Zn0.2Fe2O4/(1-x)Ba0.6Sr0.4TiO3的体积比将Ni0.8Zn0.2Fe2O4和Ba0.6Sr0.4TiO3粉体混合均匀得混合料，其中0.6≤x≤0.9；3) According to the volume ratio of xNi 0.8 Zn 0.2 Fe 2 O 4 /(1-x)Ba 0.6 Sr 0.4 TiO 3 , mix Ni 0.8 Zn 0.2 Fe 2 O 4 and Ba 0.6 Sr 0.4 TiO 3 powders evenly to obtain a mixture, where 0.6≤x≤0.9; 4)加入混合料质量份数8％～15％的PVA粘合剂造粒，经60目与120目筛网过筛，得到所需复合材料的混合粉末；所述的PVA粘合剂采用质量浓度为5％的聚乙烯醇水溶液；4) Add 8% to 15% of the PVA binder in the mass fraction of the mixture to granulate, and sieve through a 60-mesh and 120-mesh sieve to obtain the mixed powder of the required composite material; Concentration is 5% polyvinyl alcohol aqueous solution; 5)最后，将复合材料的混合粉末按需要压制成型，在550℃，保温4小时排除粘合剂PVA，再在1300～1350℃下烧结0.5～2小时成瓷，即得到具有巨介电常数和高磁导率的磁电复合材料的。5) Finally, press the mixed powder of the composite material into shape as required, heat it at 550°C for 4 hours to remove the binder PVA, and then sinter at 1300-1350°C for 0.5-2 hours to form porcelain, that is, a ceramic with a large dielectric constant is obtained. and magnetoelectric composites with high permeability. 2.一种按照权利要求1所述的具有巨介电常数和高磁导率的磁电复合材料的制备方法制成的具有巨介电常数和高磁导率的磁电复合材料，其特征在于：所述的具有巨介电常数和高磁导率的磁电复合材料的组成表达式为：xNi0.8Zn0.2Fe2O4/(1-x)Ba0.6Sr0.4TiO3，其中x为Ni0.8Zn0.2Fe2O4的体积百分数，且0.6≤x≤0.9，该复合材料在100Hz下介电常数为63000～156000，在10MHz下磁导率为5.3～29。2. a kind of magnetoelectric composite material with giant permittivity and high permeability made according to the preparation method of the magnetoelectric composite material with giant permittivity and high magnetic permeability according to claim 1, its feature In that: the composition expression of the magnetoelectric composite material with giant permittivity and high magnetic permeability is: xNi 0.8 Zn 0.2 Fe 2 O 4 /(1-x)Ba 0.6 Sr 0.4 TiO 3 , where x is The volume percentage of Ni 0.8 Zn 0.2 Fe 2 O 4 and 0.6≤x≤0.9, the dielectric constant of the composite material is 63000-156000 at 100Hz, and the magnetic permeability is 5.3-29 at 10MHz.
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Cited By (7)

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CN102211927A (en) * 2011-03-16 2011-10-12 陕西科技大学 Magnetoelectric compound material with giant dielectric constant and high saturation magnetization intensity and preparation method thereof
CN102211928A (en) * 2011-03-16 2011-10-12 陕西科技大学 Magnetoelectric composite material with huge dielectric constant and high residual magnetization strength, and preparation method thereof
CN102633501A (en) * 2012-04-25 2012-08-15 陕西科技大学 Hexagonal barium titanate base magnetoelectric composite material and preparation method thereof
CN105916814A (en) * 2014-01-17 2016-08-31 沙特基础工业全球技术公司 Development of nickel-zinc ferrites and methods for preparing same using iron-oxide byproducts of steel industry
CN109678495A (en) * 2019-01-15 2019-04-26 陕西科技大学 A kind of BaTiO3-Sr2CoMoO6Magnetoelectric ceramic and preparation method thereof
CN111298934A (en) * 2019-11-24 2020-06-19 浙江省东阳市剑华磁业有限公司 Preforming method for sintering permanent magnetic ferrite
CN112851323A (en) * 2021-01-20 2021-05-28 广州远能科技有限公司 Microwave dielectric ceramic material with high magnetic conductivity and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102211927A (en) * 2011-03-16 2011-10-12 陕西科技大学 Magnetoelectric compound material with giant dielectric constant and high saturation magnetization intensity and preparation method thereof
CN102211928A (en) * 2011-03-16 2011-10-12 陕西科技大学 Magnetoelectric composite material with huge dielectric constant and high residual magnetization strength, and preparation method thereof
CN102633501A (en) * 2012-04-25 2012-08-15 陕西科技大学 Hexagonal barium titanate base magnetoelectric composite material and preparation method thereof
CN105916814A (en) * 2014-01-17 2016-08-31 沙特基础工业全球技术公司 Development of nickel-zinc ferrites and methods for preparing same using iron-oxide byproducts of steel industry
CN109678495A (en) * 2019-01-15 2019-04-26 陕西科技大学 A kind of BaTiO3-Sr2CoMoO6Magnetoelectric ceramic and preparation method thereof
CN109678495B (en) * 2019-01-15 2021-09-07 陕西科技大学 A kind of BaTiO3-Sr2CoMoO6 magnetoelectric composite ceramic and preparation method thereof
CN111298934A (en) * 2019-11-24 2020-06-19 浙江省东阳市剑华磁业有限公司 Preforming method for sintering permanent magnetic ferrite
CN112851323A (en) * 2021-01-20 2021-05-28 广州远能科技有限公司 Microwave dielectric ceramic material with high magnetic conductivity and preparation method thereof
CN112851323B (en) * 2021-01-20 2022-01-14 新化嘉恒电子陶瓷有限责任公司 Microwave dielectric ceramic material with high magnetic conductivity and preparation method thereof

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Application publication date: 20100623