CN113087498A - High-strength high-toughness high-thermal-conductivity alumina ceramic material and preparation method and application thereof - Google Patents
High-strength high-toughness high-thermal-conductivity alumina ceramic material and preparation method and application thereof Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 33
- 239000002131 composite material Substances 0.000 claims abstract description 32
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 239000000919 ceramic Substances 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 7
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 7
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 7
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 7
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000498 ball milling Methods 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 12
- 238000002390 rotary evaporation Methods 0.000 claims description 11
- 238000009694 cold isostatic pressing Methods 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 230000003247 decreasing effect Effects 0.000 claims 1
- 238000012216 screening Methods 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 239000000306 component Substances 0.000 description 7
- 238000007789 sealing Methods 0.000 description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007676 flexural strength test Methods 0.000 description 1
- 238000007656 fracture toughness test Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses an alumina ceramic material with high strength, high toughness and high thermal conductivity, a preparation method and application thereof, and relates to the technical field of alumina ceramic materials. The alumina ceramic material is prepared from composite powder, and is characterized in that the composite powder comprises the following components in percentage by mass: al (Al)2O3‑La2O388-97.8% of composition and Nb2O51‑2％、CeO20‑6％、CaO0.5‑1％、SiO20.5-2% of MgO0.2-1%. The invention adds Nb into the lanthanum oxide doped alumina2O5、CeO2、CaO、SiO2MgO, and the density, the bending strength, the fracture toughness and the thermal conductivity of the ceramic substrate prepared by the specific sintering process are respectively not lower than 98 percent, 450MPa and 5 MPa.m1/223W/(mK). Thus, prepared by the examples of the inventionThe ceramic substrate meets the requirements of high strength, high toughness and high thermal conductivity of electronic devices, and can be widely applied to the electronic device substrate.
Description
Technical Field
The invention relates to the technical field of alumina ceramic materials, in particular to an alumina ceramic material with high strength, high toughness and high thermal conductivity, and a preparation method and application thereof.
Background
With the miniaturization, portability and multifunction of electronic productsThe development of the energy-saving direction leads the heat dissipation requirement of the electronic product to be higher and higher. As an irreplaceable key core component in the electronic information manufacturing industry, the ceramic radiating substrate plays the core maintenance roles of radiating, insulating protection and structural packaging support of various electronic components, and really plays the role of supporting the substrate of the whole electronic information manufacturing industry. Al (Al)2O3The substrate has the advantages of rich raw materials, high strength, hardness, chemical stability, thermal shock resistance and good insulativity and metal adhesiveness, is a ceramic material with better comprehensive performance and mature application in the electronic industry at present, and accounts for 90 percent of the total amount of the ceramic substrate.
But Al2O3The self-strength is not high, the bending strength is generally 280-350MPa, and La is doped2O3Can effectively improve Al2O3But at the same time, the density of the alumina is reduced and the thermal conductivity is reduced.
Disclosure of Invention
The invention aims to solve the problem of the existing doped La2O3The alumina ceramic material has the problems of low compactness and low thermal conductivity.
In order to solve the above problems, the present invention proposes the following technical solutions:
in a first aspect, an embodiment of the present invention provides an alumina ceramic material with high strength, high toughness and high thermal conductivity, where the alumina ceramic material is prepared from a composite powder, and the composite powder includes, by mass:
Al2O3-La2O388-97.8% of composition and Nb2O51-2％、CeO20-6％、CaO0.5-1％、SiO20.5-2％、MgO0.2-1％。
The further technical proposal is that Al2O3-La2O3In the composition, Al2O3And La2O3The composite powder comprises the following components in percentage by mass: al (Al)2O382-96.8％％、La2O31-7％。
In a second aspect, embodiments of the present invention provide a method for preparing a high-strength, high-toughness, high-thermal-conductivity alumina ceramic material, including:
s1, performing ball milling treatment, rotary evaporation treatment and sieving treatment on the composite powder in sequence;
s2, preparing the composite powder into a blank through a dry pressing forming process and a cold isostatic pressing process in sequence;
and S3, sintering the blank into ceramic through a sintering process.
The further technical scheme is that the technological parameters of ball milling treatment comprise: the ball milling time is 6-10 h; the rotating speed of the ball mill is 250-350 r/min; the mass ratio of the grinding balls to the grinding liquid to the composite powder is 2:2: 1.
The further technical scheme is that the technological parameters of the rotary evaporation treatment comprise: the rotary evaporation temperature is 50-60 ℃.
The further technical scheme is that the technical parameters of the sieving treatment comprise: the mesh number of the screen is 100-120 meshes.
The further technical proposal is that the pressurizing pressure is 4-6 MPa; the dwell time is 60-120 s.
The further technical proposal is that in the cold isostatic pressing process, the pressure is increased to 100-200MPa at the pressure increasing rate of 30-40MPa/min, then the pressure is maintained for 3-5min, and finally the pressure is reduced to 0MPa at the pressure reducing rate of 30-40 MPa/min.
The further technical proposal is that in the sintering process, the sintering temperature is heated to 800-.
In a third aspect, embodiments of the present invention provide a use of the high-strength, high-toughness, high-thermal-conductivity alumina ceramic material according to the first aspect in a substrate for an electronic device.
Compared with the prior art, the invention can achieve the following technical effects:
the invention adds Nb into the lanthanum oxide doped alumina2O5、CeO2、CaO、SiO2MgO, and the density, the bending strength, the fracture toughness and the thermal conductivity of the ceramic substrate prepared by the specific sintering process are respectively not less than 98 percent and 450MPa、5MPa·m1/223W/(mK). Therefore, the ceramic substrate prepared by the embodiment of the invention meets the requirements of high strength, high toughness and high thermal conductivity of electronic devices, and can be widely applied to electronic device substrates.
Detailed Description
The technical solutions in the examples will be clearly and completely described below. It is apparent that the embodiments to be described below are only a part of the embodiments of the present invention, and not all of them. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that the terms "comprises" and/or "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the embodiments of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the embodiments of the invention. As used in the description of embodiments of the present invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The embodiment of the invention provides an alumina ceramic material with high strength, high toughness and high thermal conductivity, which is prepared from composite powder, wherein the composite powder comprises the following components in percentage by mass:
Al2O3-La2O388-97.8% of composition and Nb2O51-2％、CeO20-6％、CaO0.5-1％、SiO20.5-2％、MgO0.2-1％。
Further, in Al2O3-La2O3In the composition, Al2O3And La2O3Account for the composite powderThe mass fraction of the body is: al (Al)2O382-96.8％％、La2O31-7％。
The alumina ceramic material with high strength, high toughness and high thermal conductivity can be applied to substrates of electronic devices.
The embodiment of the invention also provides a preparation method of the alumina ceramic material with high strength, high toughness and high thermal conductivity, which comprises the following steps:
and S1, performing ball milling treatment, rotary evaporation treatment and sieving treatment on the composite powder in sequence.
In the specific implementation, the technological parameters of the ball milling treatment comprise: the ball milling time is 6-10 h; the rotating speed of the ball mill is 250-350 r/min; the mass ratio of the grinding balls to the grinding liquid to the composite powder is 2:2: 1. The polishing liquid may be specifically anhydrous ethanol.
Further, the technological parameters of the rotary evaporation treatment comprise: the rotary evaporation temperature is 50-60 ℃.
Further, the process parameters of the sieving treatment include: the mesh number of the screen is 100-120 meshes.
And S2, preparing the composite powder into a blank through a dry pressing forming process and a cold isostatic pressing process in sequence.
In specific implementation, the process parameters of the dry pressing forming process comprise: the pressurizing pressure is 4-6 MPa; the dwell time is 60-120 s.
Further, in the cold isostatic pressing process, the pressurizing pressure is increased to 100-200MPa at the pressure increasing rate of 30-40MPa/min, then the pressure is maintained for 3-5min, and finally the pressure is reduced to 0MPa at the pressure reducing rate of 30-40 MPa/min.
And S3, sintering the blank into ceramic through a sintering process.
In the specific implementation, in the sintering process, the sintering temperature is raised to 800-.
The composition of the composite powder of the ceramic materials of examples 1 to 13 of the present invention by mass fraction is shown in table 1 below.
Table 1 composition table of mass fractions of composite powders in examples 1 to 13
In examples 1 to 11, the specific preparation method of the alumina ceramic material with high strength, high toughness and high thermal conductivity includes the following steps:
(1) ball milling treatment: the components of the composite powder were weighed in the proportions shown in table 1 using an electronic balance and poured into a polytetrafluoroethylene ball mill pot, followed by the addition of zirconia grinding balls and absolute ethanol, and the polytetrafluoroethylene ball mill pot containing the powder, the grinding balls and the absolute ethanol was placed into a ball mill and run at a rotation speed of 350r/min for 10 hours.
Wherein, the ball mill can be a star ball mill. The mass ratio of the grinding balls to the absolute ethyl alcohol to the composite powder is 2:2: 1.
(2) And (3) rotary steaming treatment: pouring the slurry after ball milling into a flask of a rotary evaporator, and carrying out rotary evaporation treatment at the temperature of 60 ℃ by using a rotary evaporator to remove the absolute ethyl alcohol.
(3) And (3) sieving treatment: and sieving the dried composite powder after the absolute ethyl alcohol is removed, wherein the mesh number of the sieve is 100 meshes.
(4) And dry pressing and forming process: weighing the sieved composite powder and placing the composite powder in a compression mold; and applying a pressure of 4MPa, maintaining the pressure for 60s, and then demolding to obtain a sample.
(5) And a cold isostatic pressing process: and (3) placing the dry-pressed sample in a sealing bag, sealing in vacuum, placing in a cold isostatic press, controlling the pressurizing pressure to increase to 200MPa at a pressure increasing rate of 40MPa/min, then maintaining the pressure for 5min, and finally reducing to 0MPa at a pressure reducing rate of 40 MPa/min.
(6) And the sintering process comprises the following steps: and taking the sample treated by the cold isostatic pressing process out of the vacuum sealing bag, putting the sample into a muffle furnace, raising the temperature to 1200 ℃ at the heating rate of 10 ℃/min, then raising the temperature to 1550 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2 hours, lowering the temperature to 1200 ℃ at the cooling rate of 10 ℃/min, and then cooling along with the furnace.
In examples 12 to 13, the specific preparation method of the alumina ceramic material with high strength, high toughness and high thermal conductivity includes the following steps:
(1) ball milling treatment: the components of the composite powder were weighed in the proportions shown in table 1 using an electronic balance and poured into a polytetrafluoroethylene ball mill pot, followed by the addition of zirconia grinding balls and absolute ethanol, and the polytetrafluoroethylene ball mill pot containing the powder, the grinding balls and the absolute ethanol was placed into a ball mill and run at a rotation speed of 350r/min for 10 hours.
Wherein, the ball mill can be a star ball mill. The mass ratio of the grinding balls to the absolute ethyl alcohol to the composite powder is 2:2: 1.
(2) And (3) rotary steaming treatment: pouring the slurry after ball milling into a flask of a rotary evaporator, and carrying out rotary evaporation treatment at the temperature of 60 ℃ by using a rotary evaporator to remove the absolute ethyl alcohol.
(3) And (3) sieving treatment: and sieving the dried composite powder after the absolute ethyl alcohol is removed, wherein the mesh number of the sieve is 100 meshes.
(4) And dry pressing and forming process: weighing the sieved composite powder and placing the composite powder in a compression mold; and applying a pressure of 4MPa, maintaining the pressure for 60s, and then demolding to obtain a sample.
(5) And a cold isostatic pressing process: and (3) placing the dry-pressed sample in a sealing bag, sealing in vacuum, placing in a cold isostatic press, controlling the pressurizing pressure to increase to 200MPa at a pressure increasing rate of 40MPa/min, then maintaining the pressure for 5min, and finally reducing to 0MPa at a pressure reducing rate of 40 MPa/min.
(6) And the sintering process comprises the following steps: and taking the sample subjected to the cold isostatic pressing process out of the vacuum sealing bag, putting the sample into a muffle furnace, raising the temperature to 1550 ℃ at a heating rate of 10 ℃/min, preserving the temperature for 2 hours, reducing the temperature to 1200 ℃ at a cooling rate of 10 ℃/min, and then cooling along with the furnace.
The performance of the ceramic samples of examples 1-13 are shown in Table 2, where the densification test standard is ASTMC373, the flexural strength test standard is GB/T6569-86, the thermal conductivity test standard is GB/T22588-2008, and the fracture toughness test standard is GB/T37900-2019.
TABLE 2 ceramic sample Property tables for examples 1-13
In the above examples, examples 1, 12 and 13 are comparative examples. According to the experimental data, the invention adds Nb into the lanthanum oxide doped alumina2O5、CeO2、CaO、SiO2MgO, the density, the bending strength, the fracture toughness and the thermal conductivity of the ceramic substrate prepared by a specific sintering process are respectively not lower than 98 percent, 450MPa and 5 MPa.m1/223W/(mK). Therefore, the ceramic substrate prepared by the embodiment of the invention meets the requirements of high strength, high toughness and high thermal conductivity of electronic devices, and can be widely applied to electronic device substrates.
In the above embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
While the invention has been described with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. The alumina ceramic material with high strength, high toughness and high thermal conductivity is prepared from composite powder, and is characterized in that the composite powder comprises the following components in percentage by mass:
Al2O3-La2O388-97.8% of composition and Nb2O51-2％、CeO20-6％、CaO0.5-1％、SiO20.5-2％、MgO0.2-1％。
2. High strength, high toughness, high heat in accordance with claim 1A conductive alumina ceramic material, characterized in that Al2O3-La2O3In the composition, Al2O3And La2O3The composite powder comprises the following components in percentage by mass: al (Al)2O382-96.8％％、La2O31-7％。
3. A method for preparing a high strength, high toughness and high thermal conductivity alumina ceramic material as claimed in any one of claims 1 to 2, comprising:
s1, performing ball milling treatment, rotary evaporation treatment and sieving treatment on the composite powder in sequence;
s2, preparing the composite powder into a blank through a dry pressing forming process and a cold isostatic pressing process in sequence;
and S3, sintering the blank into ceramic through a sintering process.
4. The method of claim 3, wherein the process parameters of the ball milling process comprise: the ball milling time is 6-10 h; the rotating speed of the ball mill is 250-350 r/min; the mass ratio of the grinding balls to the grinding liquid to the composite powder is 2:2: 1.
5. The method of claim 3, wherein the process parameters of the rotary evaporation treatment comprise: the rotary evaporation temperature is 50-60 ℃.
6. A method according to claim 3, wherein the process parameters of the screening process include: the mesh number of the screen is 100-120 meshes.
7. The method of claim 3, wherein the process parameters of the dry-pressing process comprise: the pressurizing pressure is 4-6 MPa; the dwell time is 60-120 s.
8. The method according to claim 3, wherein in the cold isostatic pressing process, the pressurization pressure is increased to 100-200MPa at a pressure increase rate of 30-40MPa/min, then is maintained for 3-5min, and finally is decreased to 0MPa at a pressure release rate of 30-40 MPa/min.
9. The method as claimed in claim 3, wherein the sintering temperature is raised to 800-.
10. Use of the high strength, high toughness, high thermal conductivity alumina ceramic material of any one of claims 1-2 in a substrate for an electronic device.
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