CN111498881B - Low dielectric constant alumina material for high-frequency application, preparation method and application - Google Patents

Low dielectric constant alumina material for high-frequency application, preparation method and application Download PDF

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CN111498881B
CN111498881B CN202010352278.0A CN202010352278A CN111498881B CN 111498881 B CN111498881 B CN 111498881B CN 202010352278 A CN202010352278 A CN 202010352278A CN 111498881 B CN111498881 B CN 111498881B
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dielectric constant
alumina material
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CN111498881A (en
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宋锡滨
王梦婕
王军
焦英训
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Shandong Sinocera Functional Material Co Ltd
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Abstract

The application belongs to the technical field of inorganic materials, and particularly relates to a low-dielectric-constant aluminum oxide material suitable for high-frequency application, and a preparation method and application thereof. The low dielectric constant alumina material uses aluminum ammonium sulfate as aluminum salt, uses ammonium bicarbonate as precipitator, prepares precursor basic aluminum ammonium carbonate by precipitation, and prepares alumina particles with uniform particle size by twice gradient calcination. The alumina particles of the application can be completely applied to the application fields of 5G communication consumer electronic chip packaging ceramic substrates, glass ceramic cofiring substrates and the like.

Description

Low dielectric constant alumina material for high-frequency application, preparation method and application
Technical Field
The application belongs to the technical field of inorganic materials, and particularly relates to a low-dielectric-constant aluminum oxide material suitable for high-frequency application, and a preparation method and application thereof.
Background
With the development of technology, a Printed Circuit Board (PCB) has become an indispensable electronic component. Since the 90 s of the 20 th century, printed circuit boards have been gradually changed to electronic boards (electronic substrate) worldwide, marking that conventional printed circuit boards have entered the multilayer substrate age. The materials used for the circuit board can be classified into three types, namely an inorganic board material, an organic board material and a composite board material. Wherein, the traditional inorganic substrate is mostly made of Al 2 O 3 SiC, BO, alN, etc. are used as base materials, and these materials are widely used in the MCM circuit board industry at present because they have good properties in terms of thermal conductivity, flexural strength, thermal expansion coefficient, etc.
The alumina ceramic has the advantages of high hardness, high wear resistance, high mechanical strength, high resistivity, good chemical stability, good dielectric property, good resistance to thermal shock effect, capability of forming sealed brazing with metals and the like, and the dielectric loss (tg delta) of the alumina ceramic is in a wider frequency range no matter of a polycrystalline material or a single crystal material, wherein the dielectric loss is still not large under the ultrahigh frequency condition, the change of the dielectric loss is not large along with the rise of temperature, and the relationship between the dielectric constant (epsilon) and the temperature is not obvious, so that the alumina ceramic material is a more ideal circuit substrate material.
However, there is currently hardly any relevant application in the high frequency domain for alumina ceramic products; moreover, since the dielectric constant of pure phase alpha-alumina is high, generally reaches more than 10, and is not suitable for the requirement of high-frequency application; furthermore, since the sintering temperature of pure phase α -alumina is high, it is required to reach about 1500 to 1600 ℃, and it is difficult to directly apply the pure phase α -alumina, various sintering aids are required to be added to reduce the sintering temperature of the alumina, and generally, the pure phase α -alumina contains more than 95% of Al 2 O 3 The sintering is usually carried out with the aid of a liquid phase which is formed by means of a special additive added to the batch. Therefore, most of aluminum oxide is mixed with other powder for use in the aspect of dielectric property, and the use of single-phase aluminum oxide is greatly limited.
Disclosure of Invention
Therefore, the technical problem to be solved by the application is to provide a low dielectric constant alumina material suitable for high-frequency application so as to solve the problem that the use of single-phase alumina is limited in the prior art;
the second technical problem to be solved by the present application is to provide a preparation method and application of the low dielectric constant alumina material suitable for high frequency application.
In order to solve the technical problems, the low dielectric constant alumina material for high-frequency application has the following dielectric properties:
the dielectric constant of the alumina material is 9-9.7 and Df is 0.0002-0.0008 when the frequency is 20-70 GHz.
Specifically, the specific surface of the alumina material is 10-25, the particle diameter D50 is 50-200nm, and the D90 is 200-400nm;
the green density of the dry pressed green body of the alumina material is 2.2-2.4, the density of the ceramic chip is more than 3.9, and the sintering temperature is 1200-1350 ℃.
The application also discloses a method for preparing the low dielectric constant alumina material for high-frequency application, which comprises the following steps:
(1) Taking an aluminum ammonium sulfate solution as aluminum salt, taking an ammonium bicarbonate solution as a precipitator, reacting to obtain a precursor basic aluminum ammonium carbonate, and aging the obtained precursor;
(2) Carrying out suction filtration and washing on the aged precursor, drying, and grinding for later use;
(3) Calcining the precursor powder for the first time at 700-850 ℃ to obtain transition phase gamma-Al 2 O 3 Dispersing and drying, and calcining at 1000-1100 deg.C for the second time to obtain pure phase alpha-Al 2 O 3 。
Specifically, in the step (1), the molar ratio of the aluminum ammonium sulfate to the ammonium bicarbonate is 1:8-20.
Specifically, in the step (1), the concentration of the aluminum ammonium sulfate solution is controlled to be 0.3-0.5mol/L, and the concentration of the ammonium bicarbonate solution is controlled to be 1.5-2.5mol/L.
Specifically, in the step (1), the reaction temperature is controlled to be 40-100 ℃.
Specifically, in the step (1), the temperature of the aging step is controlled to be 50-100 ℃.
Specifically, in the step (2), the temperature of the drying step is controlled to be 80-100 ℃.
Specifically, in the step (3), the dispersing step includes mixing the transition phase γ -Al 2 O 3 Adding water to prepare a solution, ball-milling for 5-10h by taking high-purity alumina balls as ball milling media, and drying and grinding the ball-milled solution.
The application also discloses application of the low dielectric constant aluminum oxide material for high-frequency application in the field of 5G high frequency.
Specifically, the application of the alumina material disclosed by the application comprises the application of preparing a ceramic substrate or a glass ceramic cofiring substrate suitable for 5G communication consumer electronic chip packaging.
The low dielectric constant alumina material uses aluminum ammonium sulfate as aluminum salt, uses ammonium bicarbonate as precipitator, prepares precursor basic aluminum ammonium carbonate by precipitation, and prepares alumina particles with uniform particle size by twice gradient calcination. The alumina particles of the application can obtain pure-phase alpha-Al after being dispersed by transition phase alumina and then calcined 2 O 3 The calcination temperature of the alumina powder prepared by the method is 1000-1100 ℃, and is reduced by 100-200 ℃ compared with that of common alumina; when the calcination temperature of alumina is lowered, the particle size of alumina particles is reduced to a minimum of about 50nm, and the dispersibility of alumina particles is more excellent. The main reason is that the alumina particles formed by common thermal decomposition are mostly adhered during growth, so that the dispersibility of the alumina particles is poor, the particles are large, the porcelain forming temperature is influenced, and the dielectric property is further influenced. The method for preparing the alumina reduces the adhesion phenomenon, improves the dispersity, reduces the particle size, reduces the ceramic forming temperature of the alumina, increases the compactness of the alumina ceramic chip and reduces the dielectric constant of the alumina by adopting the mode of dispersing and then secondarily calcining the alumina into the alumina particles.
The alumina particles of the application have a dielectric constant of 9-9.7 and a Df of 0.0002-0.0008 at 20-70GHz frequency, and can be completely applied to the application fields of 5G communication consumer electronic chip packaging ceramic substrates, glass ceramic cofiring substrates and the like.
Drawings
In order that the application may be more readily understood, a more particular description of the application will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings, in which,
FIG. 1 is an electron micrograph of a conventional alumina;
FIG. 2 is an electron micrograph of alumina prepared according to examples 1, 4, and 6 of the present application;
FIG. 3 is an electron micrograph of the alumina prepared according to comparative examples 1-2 of the present application;
FIG. 4 is an XRD pattern of alumina prepared in examples 1-7 of the application;
FIG. 5 is an XRD pattern of the alumina prepared in comparative examples 1-2 according to the present application.
Detailed Description
Example 1
The preparation method of the alumina material in the embodiment comprises the following steps:
(1) Aluminum ammonium sulfate solution (0.4 mol/L) is used as aluminum salt, ammonium bicarbonate solution (2 mol/L) is used as precipitator, and the molar ratio of aluminum ammonium sulfate to ammonium bicarbonate is controlled to be 1:15, dropwise adding the aluminum ammonium sulfate solution into the ammonium bicarbonate solution at the dropwise adding speed of 20mL/min, and reacting at 40 ℃ with stirring in the dropwise adding process to obtain a precursor basic aluminum ammonium carbonate; after the reaction is completed, stirring and ageing are carried out for 2 hours at the constant temperature of 40 ℃ while the mixture is hot;
(2) Directly carrying out suction filtration on the aged precursor, adding pure water into a filter cake after the suction filtration for pulping and washing, and repeatedly and circularly washing for 4 times; washing, drying at 100 ℃ for more than 12 hours, and grinding to obtain precursor basic ammonium aluminum carbonate powder;
(3) Calcining the precursor basic aluminum ammonium carbonate powder at 800 ℃ for 1h to obtain transition phase gamma-Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Subsequently, the transition phase gamma-Al 2 O 3 Preparing a solution with the mass concentration of 20wt%, placing the solution into a ball milling tank, performing ball milling by taking high-purity alumina balls as ball milling media so as to prevent excessive impurities from being doped, controlling the ball milling time to be 5 hours, adding alcohol into the solution after ball milling, drying, and grinding to obtain powder after drying; placing the ground powder into a medium temperature furnace, and calcining for 2 hours at 1150 ℃ to obtain pure phase alpha-Al 2 O 3 And (3) particles.
The electron micrograph shown in FIG. 2 and the XRD pattern shown in FIG. 4 show that the alumina obtained in this example is pure phase α -Al 2 O 3 The particles (see fig. 1) are small in particle size and high in dispersion degree, and the calcination temperature of the alumina particles is reduced by 100-200 ℃ compared with that of conventional alumina particles.
Example 2
The preparation method of the alumina material in the embodiment comprises the following steps:
(1) The aluminum ammonium sulfate solution (0.3 mol/L) is used as aluminum salt, the ammonium bicarbonate solution (2.5 mol/L) is used as a precipitator, and the molar ratio of aluminum ammonium sulfate to ammonium bicarbonate is controlled to be 1: dropwise adding an aluminum ammonium sulfate solution into an ammonium bicarbonate solution at a dropwise adding speed of 20mL/min, stirring during the dropwise adding process, and reacting at 60 ℃ to obtain a precursor basic aluminum ammonium carbonate; after the reaction is completed, stirring and ageing are carried out for 2 hours at the constant temperature of 60 ℃ while the mixture is hot;
(2) Directly carrying out suction filtration on the aged precursor, adding pure water into a filter cake after the suction filtration for pulping and washing, and repeatedly and circularly washing for 4 times; washing, drying at 100 ℃ for more than 12 hours, and grinding to obtain precursor basic ammonium aluminum carbonate powder;
(3) Calcining the precursor basic aluminum ammonium carbonate powder at 900 ℃ for 1h to obtain transition phase gamma-Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Subsequently, the transition phase gamma-Al 2 O 3 Preparing a solution with the mass concentration of 20wt%, placing the solution into a ball milling tank, performing ball milling by taking high-purity alumina balls as ball milling media so as to prevent excessive impurities from being doped, controlling the ball milling time to be 5 hours, adding alcohol into the solution after ball milling, drying, and grinding to obtain powder after drying; placing the ground powder into a medium temperature furnace, and calcining for 2 hours at 1100 ℃ to obtain pure phase alpha-Al 2 O 3 And (3) particles.
The XRD pattern shown in FIG. 4 shows that the alumina obtained in this example is pure phase α -Al 2 O 3 And (3) particles.
Example 3
The preparation method of the alumina material in the embodiment comprises the following steps:
(1) The aluminum ammonium sulfate solution (0.5 mol/L) is used as aluminum salt, the ammonium bicarbonate solution (1.5 mol/L) is used as a precipitator, and the molar ratio of aluminum ammonium sulfate to ammonium bicarbonate is controlled to be 1:20, dropwise adding an aluminum ammonium sulfate solution into an ammonium bicarbonate solution, wherein the dropwise adding speed is 20mL/min, stirring is carried out during the dropwise adding process, and the reaction is carried out at 80 ℃ to obtain a precursor basic aluminum ammonium carbonate; after the reaction is completed, stirring and ageing are carried out for 2 hours at the constant temperature of 80 ℃ while the mixture is hot;
(2) Directly carrying out suction filtration on the aged precursor, adding pure water into a filter cake after the suction filtration for pulping and washing, and repeatedly and circularly washing for 4 times; washing, drying at 100 ℃ for more than 12 hours, and grinding to obtain precursor basic ammonium aluminum carbonate powder;
(3) Calcining the precursor basic aluminum ammonium carbonate powder at 850 ℃ for 1h to obtain transition phase gamma-Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Subsequently, the transition phase gamma-Al 2 O 3 Preparing a solution with the mass concentration of 20wt%, placing the solution into a ball milling tank, performing ball milling by taking high-purity alumina balls as ball milling media so as to prevent excessive impurities from being doped, controlling the ball milling time to be 5 hours, adding alcohol into the solution after ball milling, drying, and grinding to obtain powder after drying; placing the ground powder into a medium temperature furnace, and calcining for 2 hours at 1100 ℃ to obtain pure phase alpha-Al 2 O 3 And (3) particles.
The XRD pattern shown in FIG. 4 shows that the alumina obtained in this example is pure phase α -Al 2 O 3 And (3) particles.
Example 4
The preparation method of the alumina material in the embodiment comprises the following steps:
(1) Aluminum ammonium sulfate solution (0.4 mol/L) is used as aluminum salt, ammonium bicarbonate solution (2 mol/L) is used as precipitator, and the molar ratio of aluminum ammonium sulfate to ammonium bicarbonate is controlled to be 1:15, dropwise adding the aluminum ammonium sulfate solution into the ammonium bicarbonate solution at the dropwise adding speed of 20mL/min, and reacting at 60 ℃ with stirring in the dropwise adding process to obtain a precursor basic aluminum ammonium carbonate; after the reaction is completed, stirring and ageing are carried out for 2 hours at the constant temperature of 80 ℃ while the mixture is hot;
(2) Directly carrying out suction filtration on the aged precursor, adding pure water into a filter cake after the suction filtration for pulping and washing, and repeatedly and circularly washing for 4 times; washing, drying at 100 ℃ for more than 12 hours, and grinding to obtain precursor basic ammonium aluminum carbonate powder;
(3) Calcining the precursor basic aluminum ammonium carbonate powder at 900 ℃ for 1h to obtain transition phase gamma-Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Subsequentlygamma-Al of transition phase 2 O 3 Preparing a solution with the mass concentration of 20wt%, placing the solution into a ball milling tank, performing ball milling by taking high-purity alumina balls as ball milling media so as to prevent excessive impurities from being doped, controlling the ball milling time for 6 hours, adding alcohol into the solution after ball milling, drying, and grinding to obtain powder after drying; placing the ground powder into a medium temperature furnace, and calcining for 2 hours at 1080 ℃ to obtain pure phase alpha-Al 2 O 3 And (3) particles.
The electron micrograph shown in FIG. 2 and the XRD pattern shown in FIG. 4 show that the alumina obtained in this example is pure phase α -Al 2 O 3 The particles have small particle size and high dispersion degree.
Example 5
The preparation method of the alumina material in the embodiment comprises the following steps:
(1) The aluminum ammonium sulfate solution (0.4 mol/L) is used as aluminum salt, the ammonium bicarbonate solution (2.5 mol/L) is used as a precipitator, and the molar ratio of aluminum ammonium sulfate to ammonium bicarbonate is controlled to be 1:14, dropwise adding the aluminum ammonium sulfate solution into the ammonium bicarbonate solution at the dropwise adding speed of 20mL/min, stirring in the dropwise adding process, and reacting at 60 ℃ to obtain a precursor basic aluminum ammonium carbonate; after the reaction is completed, stirring and ageing are carried out for 2 hours at the constant temperature of 80 ℃ while the mixture is hot;
(2) Directly carrying out suction filtration on the aged precursor, adding pure water into a filter cake after the suction filtration for pulping and washing, and repeatedly and circularly washing for 4 times; washing, drying at 100 ℃ for more than 12 hours, and grinding to obtain precursor basic ammonium aluminum carbonate powder;
(3) Calcining the precursor basic aluminum ammonium carbonate powder at 850 ℃ for 1h to obtain transition phase gamma-Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Subsequently, the transition phase gamma-Al 2 O 3 Preparing a solution with the mass concentration of 20wt%, placing the solution into a ball milling tank, performing ball milling by taking high-purity alumina balls as ball milling media so as to prevent excessive impurities from being doped, controlling the ball milling time to 7 hours, adding alcohol into the solution after ball milling, drying, and grinding to obtain powder after drying; placing the ground powder into a medium temperature furnace, and calcining at 1070 ℃ for 2 hours to obtain pure phase alpha-Al 2 O 3 And (3) particles.
The XRD pattern shown in FIG. 4 shows that the alumina obtained in this example is pure phase α -Al 2 O 3 And (3) particles.
Example 6
The preparation method of the alumina material in the embodiment comprises the following steps:
(1) The aluminum ammonium sulfate solution (0.4 mol/L) is used as aluminum salt, the ammonium bicarbonate solution (2.5 mol/L) is used as a precipitator, and the molar ratio of aluminum ammonium sulfate to ammonium bicarbonate is controlled to be 1:12, dropwise adding an aluminum ammonium sulfate solution into an ammonium bicarbonate solution at a dropwise adding speed of 20mL/min, stirring in the dropwise adding process, and reacting at 60 ℃ to obtain a precursor basic aluminum ammonium carbonate; after the reaction is completed, stirring and ageing are carried out for 2 hours at the constant temperature of 60 ℃ while the mixture is hot;
(2) Directly carrying out suction filtration on the aged precursor, adding pure water into a filter cake after the suction filtration for pulping and washing, and repeatedly and circularly washing for 4 times; washing, drying at 100 ℃ for more than 12 hours, and grinding to obtain precursor basic ammonium aluminum carbonate powder;
(3) Calcining the precursor basic aluminum ammonium carbonate powder at 850 ℃ for 1h to obtain transition phase gamma-Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Subsequently, the transition phase gamma-Al 2 O 3 Preparing a solution with the mass concentration of 20wt%, placing the solution into a ball milling tank, performing ball milling by taking high-purity alumina balls as ball milling media so as to prevent excessive impurities from being doped, controlling the ball milling time to be 8 hours, adding alcohol into the solution after ball milling, drying, and grinding to obtain powder after drying; placing the ground powder into a medium temperature furnace, and calcining for 2 hours at 1050 ℃ to obtain pure phase alpha-Al 2 O 3 And (3) particles.
The electron micrograph shown in FIG. 2 and the XRD pattern shown in FIG. 4 show that the alumina obtained in this example is pure phase α -Al 2 O 3 The particles have small particle size and high dispersion degree.
Example 7
The preparation method of the alumina material in the embodiment comprises the following steps:
(1) The aluminum ammonium sulfate solution (0.5 mol/L) is used as aluminum salt, the ammonium bicarbonate solution (2.5 mol/L) is used as a precipitator, and the molar ratio of aluminum ammonium sulfate to ammonium bicarbonate is controlled to be 1:14, dropwise adding the aluminum ammonium sulfate solution into the ammonium bicarbonate solution at the dropwise adding speed of 20mL/min, stirring in the dropwise adding process, and reacting at 60 ℃ to obtain a precursor basic aluminum ammonium carbonate; after the reaction is completed, stirring and ageing are carried out for 2 hours at the constant temperature of 60 ℃ while the mixture is hot;
(2) Directly carrying out suction filtration on the aged precursor, adding pure water into a filter cake after the suction filtration for pulping and washing, and repeatedly and circularly washing for 4 times; washing, drying at 100 ℃ for more than 12 hours, and grinding to obtain precursor basic ammonium aluminum carbonate powder;
(3) Calcining the precursor basic aluminum ammonium carbonate powder at 800 ℃ for 1h to obtain transition phase gamma-Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Subsequently, the transition phase gamma-Al 2 O 3 Preparing a solution with the mass concentration of 20wt%, placing the solution into a ball milling tank, performing ball milling by taking high-purity alumina balls as ball milling media so as to prevent excessive impurities from being doped, controlling the ball milling time to be 8 hours, adding alcohol into the solution after ball milling, drying, and grinding to obtain powder after drying; placing the ground powder into a medium temperature furnace, and calcining at 1000 ℃ for 2 hours to obtain pure phase alpha-Al 2 O 3 And (3) particles.
The XRD pattern shown in FIG. 4 shows that the alumina obtained in this example is pure phase α -Al 2 O 3 And (3) particles.
Comparative example 1
The method for preparing the alumina particles of this comparative example is the same as in example 1, except that in the step (3), the precursor basic aluminum ammonium carbonate powder is directly calcined at 800 ℃ for 3 hours.
The electron micrograph shown in FIG. 3 and the XRD pattern shown in FIG. 5 show that the alumina obtained in this comparative example is gamma-Al 2 O 3 。
Comparative example 2
The method for preparing the alumina particles of this comparative example is the same as in example 1, except that in the step (3), the precursor basic aluminum ammonium carbonate powder is directly calcined at 1050 ℃ for 3 hours.
The electron micrograph shown in FIG. 3 and the XRD pattern shown in FIG. 5 show that in this comparative exampleThe alumina obtained is gamma-Al 2 O 3 And alpha-Al 2 O 3 。
Experimental example
1. Particle size of the particles
The alumina powders prepared in examples 1 to 7 and comparative examples 1 to 2 above were subjected to performance tests, respectively, specifically comprising:
testing the specific surface value, the particle size D50 and the particle size D90 of the alumina particles;
the green density of the alumina particles dry pressed into a green body and the density of the ceramic chips after sintering at 1350 c were tested.
The test results are recorded in table 1 below.
TABLE 1 results of size Performance test of alumina particles
Numbering device Specific surface value Particle diameter D50 (mum) Particle diameter D90 (mum) Green density (g/cm) 3 ) Ceramic chip density (g/cm) 3 )
Example 1 10 0.176 0.362 2.21 3.8
Example 2 12 0.162 0.286 2.23 3.88
Example 3 14 0.158 0.215 2.24 3.9
Example 4 14.8 0.153 0.211 2.25 3.92
Example 5 15.3 0.15 0.207 2.24 3.92
Example 6 17 0.125 0.18 2.28 3.95
Example 7 20 0.1 0.163 2.3 3.96
Comparative example 1 78 0.05 0.51 2.08 3.71
Comparative example 2 46 0.07 0.42 2.02 3.75
The alumina particles prepared by the application have the specific surface between 10 and 25, the particle diameter D50 between 50 and 200nm, the D90 between 200 and 400nm, and the particles are uniform and fine; and the density of the green body of the alumina dried pressed green body is 2.2-2.4, and the density of the ceramic chip is more than 3.9.
2. Dielectric property test
Measurement of dielectric properties of alumina particles. Before testing, the material is firstly prepared into a sheet with a flat surface, and then a advanced Fabry-Perot Luo Weirao method (AFPPM method for short) developed by the company for a long time is adopted for testing.
Advanced fabry-perot Luo Weirao method: the conventional Fabry-Perot Luo Weirao method has limitation on the thickness of a sample to be tested, and cannot meet the test of samples with common thickness in the market, in order to solve the problem, the Fabry-Perot Luo Weirao method is improved according to the electromagnetic theory basis, so that the thickness range of the test sample can be expanded, and the method can be applied to more substrate materials with standard sizes in the market, and is called as a step-by-step Fabry-Perot Luo Weirao method (AdvancedFabry Perot Perturbation Methods) for short, and AFPPM method for short. The specific test process is detailed in the section 1 of the millimeter wave band material dielectric property test method of the enterprise standard Q/0500SGC003.1-2020: the dielectric constants and Df values of the alumina particles at different frequencies were measured by the method for testing dielectric properties at room temperature of 20-70GHz and are recorded in Table 2 below.
TABLE 2 dielectric property test results
Therefore, when the frequency is 20-70GHz, the dielectric constant of the alumina is 9-9.7, and Df is 0.0002-0.0008, and the alumina particles prepared by the application can be applied to the application fields of 5G communication consumer electronic chip packaging ceramic substrates, glass ceramic cofiring substrates and the like.
3. Minimum sintering temperature test
The alumina powders prepared in examples 1 to 7 and comparative examples 1 to 2 were sintered, respectively, and the minimum sintering temperature of the powders was measured, and the test results were recorded as shown in Table 3 below.
TABLE 3 minimum sintering temperature test results
Therefore, the minimum sintering temperature of the alumina particles prepared by the application is 1250-1350 ℃, the low-temperature sintering performance can effectively ensure the structural performance of the alumina particles, and the alumina particles can be applied to the application fields of 5G communication consumer electronic chip packaging ceramic substrates, glass ceramic cofiring substrates and the like.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the application.

Claims (9)

1. A low dielectric constant alumina material for high frequency applications, characterized by: the dielectric properties of the alumina material have the following properties: when the frequency is 20-70GHz, the dielectric constant of the alumina material is 9-9.7, and Df is 0.0002-0.0008;
the method of the low dielectric constant alumina material for high frequency application comprises the following steps:
(1) Taking an aluminum ammonium sulfate solution as aluminum salt, taking an ammonium bicarbonate solution as a precipitator, reacting to obtain a precursor basic aluminum ammonium carbonate, and aging the obtained precursor;
(2) Carrying out suction filtration and washing on the aged precursor, drying, and grinding for later use;
(3) Calcining the precursor powder for the first time at 700-850 ℃ to obtain transition phase gamma-Al 2 O 3 Dispersing and drying, and calcining at 1000-1100 deg.C for the second time to obtain pure phase alpha-Al 2 O 3 ;
Wherein the specific surface area of the alumina material is 10-25, the particle diameter D50 is 50-200nm, and the D90 is 200-400nm; the green density of the dry pressed green body of the alumina material is 2.2-2.4, the density of the ceramic chip is more than 3.9, and the sintering temperature is 1200-1350 ℃.
2. The low dielectric constant alumina material for high frequency applications according to claim 1, wherein in step (1), the molar ratio of the aluminum ammonium sulfate to the ammonium bicarbonate is 1:8-20.
3. The low dielectric constant alumina material for high frequency applications according to claim 1, wherein in said step (1), the concentration of said aluminum ammonium sulfate solution is controlled to be 0.3 to 0.5mol/L and the concentration of said ammonium bicarbonate solution is controlled to be 1.5 to 2.5mol/L.
4. The low dielectric constant alumina material for high frequency applications according to claim 1, wherein in said step (1), said reaction temperature is controlled to be 40-100 ℃.
5. The low dielectric constant alumina material for high frequency applications according to claim 1, wherein in said step (1), the temperature of said aging step is controlled to be 50-100 ℃.
6. The low dielectric constant alumina material for high frequency applications according to claim 1, wherein in said step (2), said drying step is controlled to a temperature of 80 to 100 ℃.
7. The high frequency application low dielectric constant alumina material as claimed in claim 1, wherein in said step (3), said dispersing step comprises subjecting said transition phase γ -Al 2 O 3 Adding water to prepare a solution, ball-milling for 5-10h by taking high-purity alumina balls as ball milling media, and drying and grinding the ball-milled solution.
8. Use of the low dielectric constant alumina material for high frequency applications according to claim 1 in the 5G high frequency domain.
9. The use according to claim 8, comprising the use of preparing a ceramic substrate or a glass ceramic cofired substrate suitable for 5G communication consumer electronics chip packaging.
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Citations (2)

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CN103496727A (en) * 2012-08-10 2014-01-08 山东大学 Preparation method for microcrystal alpha-Al2O3 aggregation
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CN104891542A (en) * 2015-06-24 2015-09-09 山东大学 Preparation method of ultrafine alpha-Al2O3 powder

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