CN106830909B - Microwave complex phase ceramic BAl2SiO6-TiO2And method for preparing the same - Google Patents

Microwave complex phase ceramic BAl2SiO6-TiO2And method for preparing the same Download PDF

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CN106830909B
CN106830909B CN201710050839.XA CN201710050839A CN106830909B CN 106830909 B CN106830909 B CN 106830909B CN 201710050839 A CN201710050839 A CN 201710050839A CN 106830909 B CN106830909 B CN 106830909B
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石锋
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Shandong University of Science and Technology
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Abstract

The invention provides a microwave complex phase ceramic BAl2SiO6‑TiO2And its preparation method, the microwave complex phase ceramic BAl2SiO6‑TiO2Has the chemical expression of (1-z) BAl2SiO6‑zTiO2Wherein, B is Ba, Sr, Ca, z is 0.05-0.25 mol ratio content; with BCO3、Al2O3、SiO2And TiO2As a raw material, according to BCO3：Al2O3：SiO2：TiO2(1-z): (1-z): (1-z): z molar ratio. The ceramic provided by the invention has excellent dielectric property, and can be used as a microwave substrate material in the millimeter wave field. The present invention has simple technological process and no pollution, and is one kind of promising microwave complex phase ceramic material.

Description

Microwave complex phase ceramic BAl2SiO6-TiO2And method for preparing the same
Technical Field
The invention relates to the field of electronic materials, in particular to microwave complex-phase ceramic BAl2SiO6-TiO2And a method for preparing the same.
Background
The microwave dielectric ceramic refers to AN information functional ceramic material which is suitable for a microwave frequency band (300 MHz-3000 GHz) and has low loss and stable temperature, is widely applied to resonators, filters, capacitors, oscillators, duplexers, dielectric waveguides, substrates, antennas and the like, is a key material of modern microwave communication technologies such as mobile communication, satellite communication, a Global Positioning System (GPS), military radar, a wireless local area network (W L AN) and the Internet of things (IOT), and has important significance for miniaturization of microwave components and improvement of selectivity of the componentsrDielectric loss tan (quality factor Q1/tan) and resonant frequency temperature coefficient τf. The high-performance microwave dielectric ceramic is different from general functional ceramic, and it has need of meeting the requirements of large relative dielectric constant, high quality factor, resonant frequency temp. coefficient close to 0 and adjustable. Therefore, we invented a new microwave complex phase ceramic BAl2SiO6-TiO2And the preparation method thereof has excellent microwave dielectric property and solves the technical problems.
Disclosure of Invention
The invention aims to provide a microwave complex phase pottery with excellent dielectric propertyThe ceramic can be used as microwave substrate material and applied to microwave complex phase ceramic BAl in the millimeter wave field2SiO6-TiO2(ii) a The second purpose is to provide microwave complex phase ceramic BAl2SiO6-TiO2And a preparation method.
One of the objects of the invention can be achieved by the following technical measures:
the microwave complex phase ceramic BAl2SiO6-TiO2Has the chemical expression of (1-z) BAl2SiO6-zTiO2Wherein, B is Ba, Sr, Ca, z is 0.05-0.25 mol ratio content; with BCO3、Al2O3、SiO2And TiO2As a raw material, according to BCO3：Al2O3：SiO2：TiO2(1-z): (1-z): (1-z): z molar ratio.
One of the objects of the invention can also be achieved by the following technical measures:
further, the raw material is BaCO3、CaCO3、SrCO3One or more of the raw materials and Al2O3、SiO2And TiO2According to BCO3：Al2O3：SiO2：TiO2The compound is prepared by mixing (1- (0.1-0.2)), (0.1-0.2) in a molar ratio.
Furthermore, the raw material is BaCO3、CaCO3、SrCO3One or more of the raw materials and Al2O3、SiO2And TiO2According to BCO3：Al2O3：SiO2：TiO2The components are mixed according to a molar ratio of 0.85:0.85:0.85: 0.15.
Further, the raw material is SrCO3：CaCO3：Al2O3：SiO2：TiO2X (1-z): 1-x) (1-z): z is mixed according to a molar ratio, wherein x is more than 0 and less than 1.
Furthermore, the raw material is BaCO3：SrCO3：Al2O3：SiO2：TiO2Y (1-z): z is mixed according to a molar ratio of more than 0 and less than 1.
Further, the raw material is CaCO3：BaCO3：Al2O3：SiO2：TiO2M (1-z): 1-m) (1-z): 1-z: (1-z): z is mixed according to a molar ratio of more than 0 and less than 1.
Further, the raw material is SrCO3：BaCO3：CaCO3：Al2O3：SiO2：TiO2X (1-z), y (1-z), m (1-z), 1-z, and (1-z): z is mixed according to a molar ratio of x to y, wherein x is more than 0 and less than 1, y is more than 0 and less than 10 and m is less than 1, and x + y + m is 1.
The second purpose of the invention can be realized by the following technical measures:
microwave complex phase ceramic BAl prepared by the above method2SiO6-TiO2The preparation method is characterized by comprising the following steps:
step 1, weighing raw materials according to a raw material ratio;
step 2, putting the raw materials obtained in the step 1 into a ball mill, adding deionized water and zirconia balls, carrying out ball milling for 4-12 hours, drying the ball-milled raw materials, and sieving to obtain powder with uniform particles;
step 3, heating the powder processed in the step 2 to 1300-1350 ℃, and preserving heat for 2-8 hours to obtain a pre-sintered material;
step 4, putting the pre-sintered material treated in the step 3 into a ball mill, adding deionized water and zirconia balls, carrying out ball milling for 4-8 hours, and finally drying the ball-milled raw materials;
step 5, adding the pre-sintered material dried in the step 4 into a polyvinyl alcohol (PVA) solution, granulating, and pressing into a green body by using a powder tablet press;
and 6, firing the blank in the air at 1400-1500 ℃ for 4-12 hours to obtain the product.
The second object of the present invention can also be achieved by the following technical measures:
further, the ball milling time in the step 2 is 6 hours; the temperature rise in the step 3 is 1320 ℃, and the temperature is kept for 4 hours; the ball milling time in the step 4 is 6 hours; the body described in step 6 was fired at 1450 ℃ for 10 hours.
Further, the microwave complex phase ceramic BAl2SiO6-TiO2The method of (1) further comprises, after step 6, testing the microwave dielectric properties of the article by a network analyzer, the tested microwave dielectric properties comprising a dielectric constantrQuality factor Qf and resonant frequency temperature coefficient tauf。
Microwave complex phase ceramic BAl2SiO6-TiO2And a preparation method thereof, belonging to the technical field of electronic materials. The ceramic is BAl2SiO6(B ═ Ba, Sr, Ca) as main phase material, and TiO2Adjusting the temperature coefficient to prepare the complex phase ceramic. In high purity BaCO3、CaCO3、SrCO3、 Al2O3、SiO2And TiO2The raw materials are subjected to ball milling, drying, sieving, polyvinyl alcohol PVA granulation, molding and degumming treatment, and then are sintered in air at 1350-1550 ℃ for 4-12 hours. The microwave complex phase ceramic material prepared by the invention has excellent dielectric property: dielectric constantr10-15 parts; qf is between 15000 and 35000, taufBetween-15 ppm/DEG C and +15 ppm/DEG C.
Drawings
FIG. 1 shows a microwave composite ceramic BAl according to the present invention2SiO6-TiO2Flow diagram of one embodiment of a method of making.
Detailed Description
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below. The formulations mentioned in the following examples are non-limiting embodiments and are only used for illustrating the present invention, and those skilled in the art can select the formulations according to the concept and material selection ratio of the present invention.
Referring to fig. 1:
in step 101, high purity BCO is applied3、Al2O3、SiO2And TiO2As a raw material, according to BCO3： Al2O3：SiO2：TiO2(1-z): (1-z): (1-z): z mol ratio proportioning and weighing raw materials
In step 102, putting the raw materials in the step 101 into a ball mill, adding deionized water and zirconia balls, and carrying out ball milling for 4-12 hours; and drying the ball-milled raw materials at 120 ℃, and sieving the dried raw materials with a 40-mesh sieve to obtain powder with uniform particles.
And 103, pre-sintering the sieved powder in the step 102 at 1300-1350 ℃, and preserving heat for 2-8 hours at the temperature.
In step 104, putting the pre-sintered material in step 103 into a ball mill, adding deionized water and zirconia balls, and carrying out ball milling for 4-8 hours; and drying the ball-milled raw materials at 120 ℃.
In step 105, adding a polyvinyl alcohol PVA solution as an adhesive for granulation after drying, sieving by a 80-mesh sieve after drying to obtain powder with uniform granules, and pressing into a green body by a powder tablet press.
And 106, firing the blank in the air at 1400-1500 ℃ for 4-12 hours to prepare the low-temperature sintered microwave composite ceramic with the small dielectric constant.
At step 107, the article is tested for microwave dielectric properties by a network analyzer. The microwave dielectric properties tested include dielectric constantrDielectric loss tan (quality factor Q1/tan) and resonant frequency temperature coefficient τf。
The ceramic provided by the invention has excellent dielectric property, and can be used as a microwave substrate material in the millimeter wave field. The invention has simple process and no pollution in the process, and is a promising microwave dielectric material. The following are several specific examples to which the present invention may be applied.
Example 1:
the microwave complex phase ceramic BAl2SiO6-TiO2Has the chemical expression of (Ba Al)2SiO6)0.75-(TiO2)0.25The preparation method comprises the following steps:
step 1, high-purity BaCO is added3、Al2O3、SiO2And TiO2As a raw material according to BaCO3： Al2O3：SiO2：TiO20.75: accurately weighing and proportioning the materials according to the molar ratio of 0.75:0.75: 0.25;
step 2, putting the raw materials obtained in the step 1 into a planetary ball mill, adding deionized water and zirconia balls, carrying out ball milling for 12 hours, drying the ball-milled raw materials in an electric heating blowing type drying box at 120 ℃, and sieving the dried powder with a 40-mesh sieve to obtain powder with uniform particles;
step 3, heating the powder material treated in the step 2 to 1300 ℃, and preserving the heat for 8 hours to obtain a pre-sintered material;
step 4, putting the pre-sintered material treated in the step 3 into a ball mill, adding deionized water and zirconia balls into a polyurethane ball mill, carrying out ball milling for 8 hours, and finally drying the ball-milled raw materials at 120 ℃;
step 5, adding the pre-sintered material dried in the step 4 into a polyvinyl alcohol (PVA) solution, granulating, drying, sieving with a 80-mesh sieve to obtain powder with uniform particles, pressing into a green body by using a powder tablet press, and pressing into a cylindrical green body with a certain size;
and 6, firing the blank in air at 1500 ℃ for 10 hours to obtain the product. After being cooled with the furnace, the dielectric property is testedr＝10；Qf＝35000，τf＝-15ppm/℃。
Example 2:
the microwave complex phase ceramic BAl2SiO6-TiO2Has the chemical expression of (Ca Al)2SiO6)0.95-(TiO2)0.05The preparation method comprises the following steps:
step 1, high purity CaCO3、Al2O3、SiO2And TiO2As raw material, according to CaCO3： Al2O3：SiO2：TiO20.95: 0.95:0.95: accurately weighing and proportioning the materials according to the molar ratio of 0.05;
step 2, putting the raw materials obtained in the step 1 into a planetary ball mill, adding deionized water and zirconia balls, carrying out ball milling for 4 hours, drying the ball-milled raw materials in an electric heating blowing type drying box at 120 ℃, and sieving the dried powder with a 40-mesh sieve to obtain powder with uniform particles;
step 3, heating the powder processed in the step 2 to 1350 ℃, and preserving heat for 2 hours to obtain a pre-sintering material;
step 4, putting the pre-sintered material treated in the step 3 into a ball mill, adding deionized water and zirconia balls into a polyurethane ball mill, carrying out ball milling for 4 hours, and finally drying the ball-milled raw materials at 120 ℃;
step 5, adding the pre-sintered material dried in the step 4 into a polyvinyl alcohol (PVA) solution, granulating, drying, sieving with a 80-mesh sieve to obtain powder with uniform particles, pressing into a green body by using a powder tablet press, and pressing into a cylindrical green body with a certain size;
and 6, firing the blank in air at 1400 ℃ for 4 hours to obtain the product. After being cooled with the furnace, the dielectric property is testedr＝15；Qf＝15000，τf＝15ppm/℃。
Example 3:
the microwave complex phase ceramic BAl2SiO6-TiO2Has the chemical expression of (Sr Al)2SiO6)0.9-(TiO2)0.1The preparation method comprises the following steps:
step 1, high-purity SrCO3、Al2O3、SiO2And TiO2As a raw material according to SrCO3： Al2O3：SiO2：TiO20.9: 0.9: 0.9: accurately weighing and proportioning the materials according to the molar ratio of 0.1;
step 2, putting the raw materials obtained in the step 1 into a planetary ball mill, adding deionized water and zirconia balls, carrying out ball milling for 6 hours, drying the ball-milled raw materials in an electric heating blowing type drying box at 120 ℃, and sieving the dried powder with a 40-mesh sieve to obtain powder with uniform particles;
step 3, heating the powder material treated in the step 2 to 1320 ℃, and preserving the heat for 4 hours to obtain a pre-sintered material;
step 4, putting the pre-sintered material treated in the step 3 into a ball mill, adding deionized water and zirconia balls into a polyurethane ball mill, carrying out ball milling for 6 hours, and finally drying the ball-milled raw materials at 120 ℃;
step 5, adding the pre-sintered material dried in the step 4 into a polyvinyl alcohol (PVA) solution, granulating, drying, sieving with a 80-mesh sieve to obtain powder with uniform particles, pressing into a green body by using a powder tablet press, and pressing into a cylindrical green body with a certain size;
and 6, firing the blank body in the air at 1450 ℃ for 10 hours to obtain the product. After being cooled with the furnace, the dielectric property is testedr＝12.4；Qf＝24654，τf＝-1.4ppm/℃。
Example 4:
the microwave complex phase ceramic BAl2SiO6-TiO2Has the chemical expression of (Sr)0.5Ca0.5Al2SiO6)0.8-(TiO2)0.2The preparation method comprises the following steps:
step 1, high-purity SrCO3、CaCO3、Al2O3、SiO2And TiO2As a raw material according to SrCO3：CaCO3：Al2O3：SiO2：TiO2Accurately weighing and proportioning materials according to the molar ratio of 0.4:0.4:0.8:0.8: 0.2;
step 2, putting the raw materials obtained in the step 1 into a planetary ball mill, adding deionized water and zirconia balls, carrying out ball milling for 5 hours, drying the ball-milled raw materials in an electric heating blowing type drying box at 120 ℃, and sieving the dried powder with a 40-mesh sieve to obtain powder with uniform particles;
step 3, heating the powder material treated in the step 2 to 1320 ℃, and preserving the heat for 6 hours to obtain a pre-sintered material;
step 4, putting the pre-sintered material treated in the step 3 into a ball mill, adding deionized water and zirconia balls into a polyurethane ball mill, carrying out ball milling for 5 hours, and finally drying the ball-milled raw materials at 120 ℃;
step 5, adding the pre-sintered material dried in the step 4 into a polyvinyl alcohol (PVA) solution, granulating, drying, sieving with a 80-mesh sieve to obtain powder with uniform particles, pressing into a green body by using a powder tablet press, and pressing into a cylindrical green body with a certain size;
and 6, firing the blank body in air at 1450 ℃ for 6 hours to obtain the product. After being cooled with the furnace, the dielectric property is testedr＝12.9；Qf＝22894，τf＝-11.4ppm/℃。
Example 5:
the microwave complex phase ceramic BAl2SiO6-TiO2Has the chemical expression of (Ba)0.8Sr0.2Al2SiO6)0.85-(TiO2)0.15The preparation method comprises the following steps:
step 1, high-purity BaCO is added3、SrCO3、Al2O3、SiO2And TiO2As a raw material according to BaCO3：SrCO3：Al2O3：SiO2：TiO2Accurately weighing and proportioning materials according to the molar ratio of 0.68:0.17:0.85:0.85: 0.15;
step 2, putting the raw materials obtained in the step 1 into a planetary ball mill, adding deionized water and zirconia balls, carrying out ball milling for 5 hours, drying the ball-milled raw materials in an electric heating blowing type drying box at 120 ℃, and sieving the dried powder with a 40-mesh sieve to obtain powder with uniform particles;
step 3, heating the powder material treated in the step 2 to 1340 ℃, and preserving heat for 6 hours to obtain a pre-sintered material;
step 4, putting the pre-sintered material treated in the step 3 into a ball mill, adding deionized water and zirconia balls into a polyurethane ball mill, carrying out ball milling for 6 hours, and finally drying the ball-milled raw materials at 120 ℃;
step 5, adding the pre-sintered material dried in the step 4 into a polyvinyl alcohol (PVA) solution, granulating, drying, sieving with a 80-mesh sieve to obtain powder with uniform particles, pressing into a green body by using a powder tablet press, and pressing into a cylindrical green body with a certain size;
step 6, putting the blank in air at 1Firing for 4 hours at 420 ℃ to obtain the product. After being cooled with the furnace, the dielectric property is testedr＝14.2；Qf＝15750，τf＝3.4ppm/℃。
Example 6:
the microwave complex phase ceramic BAl2SiO6-TiO2Has the chemical expression of (Sr)0.4Ba0.4Ca0.2Al2SiO6)0.8-(TiO2)0.2The preparation method comprises the following steps:
step 1, high-purity SrCO3、BaCO3、CaCO3、Al2O3、SiO2And TiO2As a raw material according to SrCO3：BaCO3：CaCO3：Al2O3：SiO2：TiO2Accurately weighing and proportioning materials according to the molar ratio of 0.32:0.32:0.16:0.8: 0.2;
step 2, putting the raw materials obtained in the step 1 into a planetary ball mill, adding deionized water and zirconia balls, carrying out ball milling for 6 hours, drying the ball-milled raw materials in an electric heating blowing type drying box at 120 ℃, and sieving the dried powder with a 40-mesh sieve to obtain powder with uniform particles;
step 3, heating the powder material treated in the step 2 to 1310 ℃, and preserving the heat for 6 hours to obtain a pre-sintered material;
step 4, putting the pre-sintered material treated in the step 3 into a ball mill, adding deionized water and zirconia balls into a polyurethane ball mill, carrying out ball milling for 5 hours, and finally drying the ball-milled raw materials at 120 ℃;
step 5, adding the pre-sintered material dried in the step 4 into a polyvinyl alcohol (PVA) solution, granulating, drying, sieving with a 80-mesh sieve to obtain powder with uniform particles, pressing into a green body by using a powder tablet press, and pressing into a cylindrical green body with a certain size;
and 6, firing the blank in air at 1420 ℃ for 5 hours to obtain the product. After being cooled with the furnace, the dielectric property is testedr＝14.2；Qf＝17800，τf＝13.6ppm/℃。
The above description is only an embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the protection scope of the present invention.

Claims (7)

1. Microwave complex phase ceramic BAl2SiO6-TiO2It is characterized in that the microwave complex phase ceramic BAl2SiO6-TiO2Has the chemical expression of (1-z) BAl2SiO6-zTiO2Wherein, B is Ba, Sr, Ca, z is 0.05-0.25 mol ratio content; with BCO3、Al2O3、SiO2And TiO2As a raw material, according to BCO3：Al2O3：SiO2：TiO2(1-z): (1-z): (1-z): z molar ratio.
2. The microwave composite ceramic BAl of claim 12SiO6-TiO2The method is characterized in that the raw material is BaCO3、CaCO3、SrCO3One or more of the raw materials and Al2O3、SiO2And TiO2According to BCO3：Al2O3：SiO2：TiO2The compound is prepared by mixing (1- (0.1-0.2)), (0.1-0.2) in a molar ratio.
3. The microwave composite ceramic BAl of claim 12SiO6-TiO2The method is characterized in that the raw material is BaCO3、CaCO3、SrCO3One or more of the raw materials and Al2O3、SiO2And TiO2According to BCO3：Al2O3：SiO2：TiO2The components are mixed according to a molar ratio of 0.85:0.85:0.85: 0.15.
4. The microwave composite ceramic according to claim 1BAl2SiO6-TiO2The method is characterized in that the raw material is CaCO3：BaCO3：Al2O3：SiO2：TiO2M (1-z): 1-m) (1-z): 1-z: (1-z): z is mixed according to a molar ratio of more than 0 and less than 1.
5. The microwave composite ceramic BAl of any one of claims 1-42SiO6-TiO2The preparation method is characterized by comprising the following steps:
step 1, weighing raw materials according to a raw material ratio;
step 2, putting the raw materials obtained in the step 1 into a ball mill, adding deionized water and zirconia balls, carrying out ball milling for 4-12 hours, drying the ball-milled raw materials, and sieving to obtain powder with uniform particles;
step 3, heating the powder processed in the step 2 to 1300-1350 ℃, and preserving heat for 2-8 hours to obtain a pre-sintered material;
step 4, putting the pre-sintered material treated in the step 3 into a ball mill, adding deionized water and zirconia balls, carrying out ball milling for 4-8 hours, and finally drying the ball-milled raw materials;
step 5, adding the pre-sintered material dried in the step 4 into a polyvinyl alcohol PVA solution, granulating, and pressing into a green body by using a powder tablet press;
and 6, firing the blank in the air at 1400-1500 ℃ for 4-12 hours to obtain the product.
6. The microwave composite ceramic BAl of claim 52SiO6-TiO2The preparation method of (1) is characterized in that the ball milling time in the step (2) is 6 hours; the temperature rise in the step 3 is 1320 ℃, and the temperature is kept for 4 hours; the ball milling time in the step 4 is 6 hours; the body described in step 6 was fired at 1450 ℃ for 10 hours.
7. The microwave composite ceramic BAl of claim 52SiO6-TiO2A process for the preparation ofIs characterized in that the microwave complex phase ceramic BAl2SiO6-TiO2The method of (1) further comprises, after step 6, testing the microwave dielectric properties of the article by a network analyzer, the tested microwave dielectric properties comprising a dielectric constantrQuality factor Qf and resonant frequency temperature coefficient tauf。
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08301651A (en) * 1995-04-28 1996-11-19 Kyocera Corp Glass-ceramic sintered material and its production
CN101851088A (en) * 2009-03-30 2010-10-06 京瓷株式会社 Dielectric ceramics and dielectric resonator
KR20140036090A (en) * 2012-09-14 2014-03-25 부산대학교 산학협력단 Dye-sensitized solar cell including phosphorescent particle

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08301651A (en) * 1995-04-28 1996-11-19 Kyocera Corp Glass-ceramic sintered material and its production
CN101851088A (en) * 2009-03-30 2010-10-06 京瓷株式会社 Dielectric ceramics and dielectric resonator
KR20140036090A (en) * 2012-09-14 2014-03-25 부산대학교 산학협력단 Dye-sensitized solar cell including phosphorescent particle

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