阅读说明：本技术 一种玻璃陶瓷材料及其制备方法和应用 (Glass ceramic material and preparation method and application thereof ) 是由 丁书强 郭金明 野田悟 唐勇 范盛东 张梦婷 于 2020-06-12 设计创作，主要内容包括：本发明公开了一种玻璃陶瓷材料,其为(Mg<Sub>1－x</Sub>X<Sub>x</Sub>)<Sub>2</Sub>Al<Sub>4</Sub>Si<Sub>5</Sub>O<Sub>18</Sub>体系微波陶瓷材料,其中X为贱金属,通过加入贱金属,获得了一种高品质因素、低介电常数的玻璃陶瓷材料,提高信号传输速度,降低材料在使用过程中对电厂的削弱,同时大大降低能量损耗。采用本申请方法制备得到的玻璃陶瓷材料的介电常数范围能够达到4.6-5.0；品质因数范围能够达到50000GHz-200000GHz；频率温度系数能够达到4.3ppm/℃～5.4ppm/℃。(The invention discloses a glass ceramic material which is (Mg) 1－x X x ) 2 Al 4 Si 5 O 18 The microwave ceramic material system is a glass ceramic material with high quality factor and low dielectric constant, wherein X is base metal, and the glass ceramic material with high quality factor and low dielectric constant is obtained by adding the base metal, so that the signal transmission speed is improved, the weakening of the material to a power plant in the using process is reduced, and the energy loss is greatly reduced. The dielectric constant range of the glass ceramic material prepared by the method can reach 4.6-5.0; the quality factor range can reach 50000GHz-200000 GHz; the temperature coefficient of frequency can reach 4.3 ppm/DEG C to 5.4 ppm/DEG C.)

1. A glass-ceramic material characterized by: the glass ceramic material is (Mg 1)_－xX_x)₂Al₄Si₅O₁₈And (4) preparing the system.

2. The glass-ceramic material of claim 1, wherein: in the structural formula, X is base metal.

3. The glass-ceramic material of claim 1, wherein: in the structural formula, Mg_1－xWherein x is in the range of 0.01 to 0.1.

4. The glass-ceramic material of claim 1, wherein: the dielectric constant of the glass ceramic material ranges from 4.6 to 5.0; the quality factor range is 50000GHz-200000 GHz; the temperature coefficient of frequency is 4.3 ppm/DEG C to 5.4 ppm/DEG C.

5. A method for the preparation of a glass-ceramic material according to any of claims 1 to 4, characterized in that: the method comprises the following steps:

1) MgO and Al with the purity of more than 99.9 percent₂O₃、SiO₂And X metal according to the stoichiometric formula (Mg)_1－xX_x)₂Al₄Si₅O₁₈X is more than or equal to 0.1 and less than or equal to 1, and the mixture is obtained after weighing and mixing;

2) putting the mixture obtained in the step 1) into a planetary ball mill for wet ball milling for 20-24 h to obtain mixed slurry powder;

3) putting the mixed slurry obtained in the step 2) into an oven, and drying the mixed slurry to constant weight at the temperature of 80-100 ℃ to obtain mixed dry powder;

4) passing the mixed dry powder obtained in the step 3) through a 60-mesh standard sieve, and then placing the powder into a high-temperature furnace for pre-burning for 4 hours to enable the mixture to react preliminarily to synthesize a pre-burnt material;

5) placing the pre-sintered material obtained in the step 4) into a planetary ball mill for ball milling, and then calcining at the temperature of 1000-1100 ℃ to obtain a calcined material;

6) putting the calcined material obtained in the step 6) into a platinum crucible for melting, wherein the melting temperature is 1500-1600 ℃, clarifying at 1500-1600 ℃ for 0.5-2 hours, and then putting into clear water for cooling;

7) placing the cooled material in the step 6) into a planetary ball mill for ball milling to microspheres with the diameter of 1-3 mm;

8) Crystallizing the microspheres obtained in the step 7) at 1000-1200 ℃, and ball-milling the obtained crystals in a planetary ball mill to obtain powder with the diameter of 1-5 μm to obtain the glass ceramic material.

6. The method of preparing a glass-ceramic material according to claim 5, wherein: the X metal in the step 1) is one of base metals.

7. The method of preparing a glass-ceramic material according to claim 5, wherein: the pre-sintering temperature in the step 4) is 1400 ℃, the calcining temperature in the step 5) is 1000 ℃, the melting temperature in the step 6) is 1550 ℃, the clarifying temperature in the step 6) is 1600 ℃, and the crystallization temperature in the step 8) is 1000 ℃.

8. The method of preparing a glass-ceramic material according to claim 5, wherein: the diameter of the microsphere in the step 7) is 1mm, and the diameter of the powder in the step 8) is 100 mu m.

9. Use of a glass-ceramic material according to any one of claims 1 to 8, characterized in that: the glass ceramic material is applied to the field of 5G communication.

Technical Field

The invention belongs to the technical field of electronic communication materials, and particularly relates to a glass ceramic material and a preparation method and application thereof.

Background

With the development of the mobile internet, more and more devices are accessed into the mobile network, new services and applications are in endless, global mobile broadband users are expected to reach 90 billion in 2018, and the capacity of the mobile communication network is expected to increase 1000 times on the current network capacity by 2020. The explosion of mobile data traffic will present a serious challenge to the network. Firstly, if the capacity is hard to support the thousand times of flow increase according to the development of the current mobile communication network, the network energy consumption and the bit cost are hard to bear; secondly, the further demand on the frequency spectrum is brought by the increase of the flow, and the mobile communication frequency spectrum is scarce, so that the available frequency spectrum is in large-span and fragmented distribution, and the efficient use of the frequency spectrum is difficult to realize; in addition, to increase network capacity, network resources must be intelligently and efficiently utilized, for example, intelligent optimization is performed for services and the personality of a user, but the capacity in this respect is insufficient; finally, the future network is inevitably a heterogeneous mobile network with multiple networks, and to improve the network capacity, the problems of efficiently managing each network, simplifying the interoperation, and enhancing the user experience must be solved. In order to solve the above challenges and meet the increasing mobile traffic demand, the development of a new generation of 5G mobile communication network is urgently needed.

And the development of the 5G mobile communication network relies on the upgrade progress of the communication devices as a support.

Microwave circuits used in communication devices generally consist of elements such as resonators, filters, oscillators, attenuators, dielectric antennas, microwave integrated circuit substrates, and the like, and microwave dielectric ceramics are key basic materials for preparing corresponding advanced electronic components. Among the above elements, glass-ceramic is the most core raw material, and its dielectric constant, which is the product of relative dielectric constant and absolute dielectric constant in vacuum, quality factor Qf and temperature coefficient of frequency τ f are all very important physical parameters. If a material with a high dielectric constant is placed in an electric field, the strength of the electric field will drop appreciably within the dielectric. The relative dielectric constant of an ideal conductor is infinite; the quality factor represents a quality index of the ratio of the energy stored in an energy storage device (such as an inductance coil, a capacitance and the like) and the energy lost per week of a resonant circuit. The greater the Q value of the element, the better the selectivity of the circuit or network formed by the element. The ceramic material with low dielectric constant and high quality factor can be used as a resonator, a filter, a microwave wire and other components in a microwave millimeter communication information system to improve the performance of the components.

Glass medium ceramics (also called microcrystalline glass) is a composite material which is prepared by high-temperature melting, molding and heat treatment and combines a crystal phase with glass. Has the advantages of high mechanical strength, adjustable thermal expansion performance, thermal shock resistance, chemical corrosion resistance, low dielectric loss and the like, and is commonly used as electronic devices. The dielectric constant of the glass ceramic communication material commonly used in the market is usually between 4 and 7, and the quality factor is between 10000-50000. The researchers in this field are working on finding glass-ceramic materials with relatively low dielectric factors and at the same time high quality factors.

Disclosure of Invention

In view of the above disadvantages, the present invention provides a glass-ceramic material having a relatively low dielectric constant and a high quality factor.

In order to realize the purpose, the following specific technical scheme is adopted:

a glass-ceramic material, which is (Mg)_1－xX_x)₂Al₄Si₅O₁₈And in the structural formula, X is base metal. In the structural formula, Mg_1－xWherein x is in the range of 0.01 to 0.1.

The dielectric constant of the glass ceramic material ranges from 4.6 to 5.0; the quality factor range is 50000GHz-200000 GHz; the temperature coefficient of frequency tau f is 4.3 ppm/DEG C to 5.4 ppm/DEG C.

A preparation method of a glass ceramic material comprises the following steps:

1) MgO and Al with the purity of more than 99.9 percent₂O₃、SiO₂And X metal according to the stoichiometric formula (Mg)_1－xX_x)₂Al₄Si₅O₁₈X is more than or equal to 0.1 and less than or equal to 1, and the mixture is obtained after weighing and mixing;

2) putting the mixture obtained in the step 1) into a planetary ball mill for wet ball milling for 20-24 h to obtain mixed slurry powder;

3) putting the mixed slurry obtained in the step 2) into an oven, and drying the mixed slurry to constant weight at the temperature of 80-100 ℃ to obtain mixed dry powder;

4) passing the mixed dry powder obtained in the step 3) through a 60-mesh standard sieve, and then placing the powder into a high-temperature furnace for pre-burning for 4 hours to enable the mixture to react preliminarily to synthesize a pre-burnt material;

5) placing the pre-sintered material obtained in the step 4) into a planetary ball mill for ball milling, and then calcining at the temperature of 1000-1100 ℃ to obtain a calcined material;

6) putting the calcined material obtained in the step 6) into a platinum crucible for melting, wherein the melting temperature is 1500-1600 ℃, clarifying at 1500-1600 ℃ for 0.5-2 hours, and then putting into clear water for cooling;

7) placing the cooled material in the step 6) into a planetary ball mill for ball milling to microspheres with the diameter of 1-3 mm;

8) crystallizing the microspheres obtained in the step 7) at 1000-1200 ℃, and ball-milling the obtained crystals in a planetary ball mill to obtain powder with the diameter of 1-5 μm to obtain the glass ceramic material.

Preferably, the X metal in step 1) is one of base metals.

Preferably, the pre-sintering temperature in the step 4) is 1400 ℃, the calcining temperature in the step 5) is 1000 ℃, the melting temperature in the step 6) is 1550 ℃, the clarifying temperature in the step 6) is 1600 ℃, and the crystallization temperature in the step 8) is 1000 ℃.

Preferably, the diameter of the microspheres in the step 7) is 1mm, and the diameter of the powder in the step 8) is 100 μm.

The application of the glass ceramic material comprises the following specific steps: the glass ceramic material is applied to the field of 5G communication.

Compared with the prior art, the glass ceramic material has the following beneficial effects:

1. in the preparation process of the material, base metal is added to obtain the glass ceramic material with high quality factor and low dielectric constant, so that the signal transmission speed is improved, the weakening of the material to a power plant in the use process is reduced, and the energy loss is greatly reduced.

2. In the preparation process, a multiple grinding process is adopted, so that the particle size of the material is gradually reduced to micron level, particle agglomeration is prevented, and the particle size is more uniform.

3. The invention can be applied to various electronic elements such as resonators, filters and the like, and has the advantages of small volume, light weight, convenient maintenance in the use process and wider application compared with other high-quality-factor materials.

Drawings

FIG. 1 shows (Mg) prepared in example 1 of the present invention_0.9Cu_0.1)₂Al₄Si₅O₁₈Scanning electron microscope photomicrograph of the glass ceramic material.

Detailed Description

The present invention will be described in further detail by way of specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.