CN115784750A - High-density aluminum nitride ceramic and preparation method thereof - Google Patents
High-density aluminum nitride ceramic and preparation method thereof Download PDFInfo
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- CN115784750A CN115784750A CN202211604711.0A CN202211604711A CN115784750A CN 115784750 A CN115784750 A CN 115784750A CN 202211604711 A CN202211604711 A CN 202211604711A CN 115784750 A CN115784750 A CN 115784750A
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 55
- 239000000919 ceramic Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000003825 pressing Methods 0.000 claims abstract description 32
- 238000005245 sintering Methods 0.000 claims abstract description 32
- 239000011812 mixed powder Substances 0.000 claims abstract description 27
- 238000000498 ball milling Methods 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 15
- 230000009471 action Effects 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000007873 sieving Methods 0.000 claims description 10
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 9
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 9
- 229940105963 yttrium fluoride Drugs 0.000 claims description 9
- RBORBHYCVONNJH-UHFFFAOYSA-K yttrium(iii) fluoride Chemical compound F[Y](F)F RBORBHYCVONNJH-UHFFFAOYSA-K 0.000 claims description 9
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 8
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 8
- 238000005452 bending Methods 0.000 claims description 7
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 10
- 238000000280 densification Methods 0.000 abstract description 7
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 17
- 239000002245 particle Substances 0.000 description 13
- 238000000227 grinding Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008707 rearrangement Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention provides high-density aluminum nitride ceramic and a preparation method thereof, belonging to the technical field of ceramic materials, wherein the preparation method of the aluminum nitride ceramic comprises the following steps: s1, carrying out ball milling and mixing on nano aluminum nitride powder, a sintering aid and a solvent to obtain mixed powder; s2, pre-pressing the mixed powder to obtain a pre-pressed body; and S3, sintering the pre-pressing body under the action of dynamic pressure and ultrasonic wave to obtain the aluminum nitride ceramic. The preparation method provided by the invention has simple process, can realize the rapid densification of the material at a lower temperature, and can prepare the aluminum nitride ceramic with high density, low defect, high strength and high thermal conductivity.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to high-density aluminum nitride ceramic and a preparation method thereof.
Background
The aluminum nitride ceramic has high thermal conductivity (theoretical thermal conductivity of 320W/m.K), relatively low dielectric constant and dielectric loss, and thermal expansion coefficient (thermal expansion coefficient of about 3.5-4.8 × 10) matched with chip materials such as silicon and gallium arsenide - 6 K -1 ) The ceramic material has a series of excellent performances such as no toxicity and insulation, is considered to be the first choice material of a new generation of high-performance ceramic heat dissipation device, and is widely applied to the fields of electronics, automobiles, aerospace, military, national defense and the like.
The sintering process in the preparation process of the aluminum nitride ceramic is a key step for realizing particle densification and endowing the material with mechanical strength and performance; the conventional sintering method is easy to generate the phenomena of hard agglomeration and micro-unevenness in the sintering process, the sintering densification is difficult to realize, and the aluminum nitride ceramic with high density, high strength and high thermal conductivity cannot be obtained.
Disclosure of Invention
The preparation method provided by the invention has simple process, can realize the rapid densification of the material at lower temperature, and can prepare the aluminum nitride ceramic with high density, low defect, high strength and high thermal conductivity.
The invention provides a preparation method of high-density aluminum nitride ceramic in a first aspect, which comprises the following steps:
s1, carrying out ball milling and mixing on nano aluminum nitride powder, a sintering aid and a solvent to obtain mixed powder;
s2, performing pre-pressing treatment on the mixed powder to obtain a pre-pressed body;
s3, sintering the pre-pressing body under the action of dynamic pressure and ultrasonic waves to obtain the aluminum nitride ceramic; applying the dynamic pressure in a thickness direction of the pre-compact; the ultrasonic waves are applied in a direction perpendicular to the thickness of the pre-compact.
Preferably, the mass ratio of the nano aluminum nitride powder to the sintering aid is (90-98) to (2-10).
Preferably, the sintering aid is one or more of yttrium fluoride, calcium fluoride and magnesium fluoride;
the solvent is absolute ethyl alcohol.
Preferably, the method further comprises the steps of drying and screening after the ball milling and mixing.
Preferably, the pressure of the pre-pressing treatment is 5 to 20MPa.
Preferably, the dynamic pressure is in the range of 30 +/-5 MPa to 50 +/-10 MPa; the frequency of the dynamic pressure is 1-5 Hz.
Preferably, the frequency of the ultrasonic wave is 20KHz.
Preferably, the sintering treatment is to heat up to 1500-1600 ℃ at a heating rate of 10-20 ℃/min.
The invention provides high-density aluminum nitride ceramic in a second aspect, which is prepared by the preparation method in the first aspect.
Preferably, the density of the aluminum nitride ceramic is not less than 99.4%, the thermal conductivity is not less than 100W/m.K, and the bending strength is not less than 500MPa.
Compared with the prior art, the invention at least has the following beneficial effects:
the invention applies dynamic pressure along the thickness direction of the pre-pressing body, applies ultrasonic wave along the direction vertical to the thickness direction of the pre-pressing body, couples the ultrasonic wave permeation technology and the dynamic pressure sintering method, can accelerate the movement of particles, promotes the slippage and rearrangement, flow mass transfer, air hole diffusion and elimination of the particles, eliminates 'hard agglomeration' to a greater extent, reduces the micro-nonuniform phenomenon of the material, realizes the rapid densification of the material at a lower temperature, improves the powder bulk density, promotes the air hole discharge, thereby preparing the aluminum nitride ceramic material with high density, low defect, high strength and high heat conductivity.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer and more complete, the following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without creative efforts based on the embodiments of the present invention belong to the protection scope of the present invention.
The invention provides a preparation method of high-density aluminum nitride ceramic in a first aspect, which comprises the following steps:
s1, carrying out ball milling and mixing on nano aluminum nitride powder, a sintering aid and a solvent to obtain mixed powder;
s2, performing pre-pressing treatment on the mixed powder to obtain a pre-pressed body;
s3, sintering the pre-pressing body under the action of dynamic pressure and ultrasonic waves to obtain the aluminum nitride ceramic; applying the dynamic pressure in a thickness direction of the pre-compact; the ultrasonic waves are applied in a direction perpendicular to the thickness of the pre-compact.
The invention applies dynamic pressure along the thickness direction of the pre-pressing body, applies ultrasonic pulse along the direction vertical to the thickness direction of the pre-pressing body, couples the ultrasonic penetration technology and the dynamic pressure sintering method, can accelerate the movement of particles, promotes the slippage and rearrangement, flow mass transfer, air hole diffusion and elimination of the particles, eliminates 'hard agglomeration' to a greater extent, reduces the micro-nonuniform phenomenon of the material, realizes the rapid densification of the material at a lower temperature, improves the powder bulk density, promotes the air hole exhaust, thereby preparing the aluminum nitride ceramic material with high density, low defect, high strength and high thermal conductivity.
According to some preferred embodiments, the mass ratio of the aluminum nitride nanopowder to the sintering aid is (90-98) - (2-10) (e.g., can be 90.
According to some preferred embodiments, the sintering aid is one or more of yttrium fluoride, calcium fluoride, magnesium fluoride; the solvent is absolute ethyl alcohol.
According to some preferred embodiments, the method further comprises the steps of drying and screening after the ball milling and mixing.
The method comprises the steps of mixing aluminum nitride nanopowder and a sintering aid by a wet ball milling method, taking high-purity zirconia balls as a grinding medium, drying after ball milling and uniform mixing, and sieving with a 200-mesh sieve to obtain mixed powder.
According to some preferred embodiments, the pressure of the pre-pressing treatment is 5 to 20MPa.
The mixed powder is put into a sintering furnace and is applied with pressure of 5-20 MPa to carry out pre-pressing treatment on the mixed powder, so as to obtain a pre-pressing body for preliminary forming.
According to some preferred embodiments, the dynamic pressure ranges from 30 ± 5MPa to 50 ± 10MPa; the dynamic pressure is applied at a frequency of 1 to 5Hz (e.g., may be 1Hz, 2Hz, 3Hz, 4Hz, or 5 Hz).
It should be noted that the dynamic pressure of the invention is a sinusoidal dynamic pressure, the pressure change of which satisfies a sinusoidal waveform, and the frequency of applying the dynamic pressure is the number of times that the pressure is from the maximum value to the minimum value within 1 s; taking the dynamic pressure of 30 +/-5 MPa as an example, the maximum value of the sine waveform is 35MPa, and the minimum value is 25MPa; the frequency of the dynamic pressure application is the number of times that the pressure is from 35MPa to 25MPa within 1 s.
According to some preferred embodiments, the frequency of the ultrasonic waves is 20KHz.
According to some preferred embodiments, the sintering treatment is carried out at a temperature rise rate of 10-20 ℃/min to 1500-1600 ℃ (for example, 1500 ℃, 1520 ℃, 1540 ℃, 1560 ℃, 1580 ℃ or 1600 ℃) and at a temperature of 2-8 h (for example, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h, 6h, 6.5h, 7h, 7.5h or 8 h).
The invention provides high-density aluminum nitride ceramic in a second aspect, which is prepared by the preparation method in the first aspect.
According to some preferred embodiments, the aluminum nitride ceramic has a compactness of not less than 99.4%, a thermal conductivity of not less than 100W/m · K, and a bending strength of not less than 500MPa.
In order to more clearly illustrate the technical solutions and advantages of the present invention, the present invention is further described below with reference to the following embodiments.
The materials and reagents in the invention can be obtained by direct purchase or self-synthesis on the market, and the specific model is not limited.
Example 1
S1, performing wet ball milling and mixing on 500g of nano aluminum nitride powder (with the particle size of 50 nm), 10g of yttrium fluoride, 10g of calcium fluoride, 10g of magnesium fluoride and absolute ethyl alcohol, wherein a grinding medium is high-purity zirconia balls, and drying and sieving to obtain mixed powder after ball milling and mixing uniformly;
s2, putting the mixed powder into a sintering furnace, and performing pre-pressing treatment under the pressure of 10MPa to obtain a pre-pressed body;
and S3, simultaneously applying dynamic pressure (the pressure is 50 +/-10 MPa and the frequency is 2 Hz) and ultrasonic waves (the frequency is 20 KHz) to the pre-pressing body, heating to 1600 ℃ at the heating rate of 20 ℃/min, and preserving heat for 6h to obtain the aluminum nitride ceramic.
The aluminum nitride ceramic prepared in example 1 has a density of 99.8%, a thermal conductivity of 130W/m.K, and a flexural strength of 650MPa.
Example 2
S1, performing wet ball milling and mixing on 500g of nano aluminum nitride powder (with the particle size of 50 nm), 30g of yttrium fluoride and absolute ethyl alcohol, wherein a grinding medium is high-purity zirconia balls, and drying and sieving to obtain mixed powder after ball milling and mixing uniformly;
s2, putting the mixed powder into a sintering furnace, and performing pre-pressing treatment under the pressure of 10MPa to obtain a pre-pressed body;
s3, simultaneously applying dynamic pressure (the pressure is 40 +/-10 MPa and the frequency is 4 Hz) and ultrasonic waves (the frequency is 20 KHz) to the pre-pressing body, heating to 1550 ℃ at the heating rate of 20 ℃/min, and preserving heat for 8 hours to obtain the aluminum nitride ceramic.
The compactness of the aluminum nitride ceramic prepared in the example 2 reaches 99.5%, the thermal conductivity is 110W/m.K, and the bending strength is 530MPa.
Example 3
S1, performing wet ball milling and mixing on 500g of nano aluminum nitride powder (with the particle size of 50 nm), 30g of calcium fluoride and absolute ethyl alcohol, wherein a grinding medium is high-purity zirconia balls, and drying and sieving to obtain mixed powder after ball milling and mixing uniformly;
s2, putting the mixed powder into a sintering furnace, and performing pre-pressing treatment under the pressure of 10MPa to obtain a pre-pressed body;
s3, simultaneously applying dynamic pressure (the pressure is 30 +/-5 MPa and the frequency is 5 Hz) and ultrasonic waves (the frequency is 20 KHz) to the pre-pressing body, heating to 1500 ℃ at the heating rate of 20 ℃/min, and preserving heat for 4h to obtain the aluminum nitride ceramic.
The aluminum nitride ceramic prepared in example 3 had a densification degree of 99.4%, a thermal conductivity of 105W/m.K, and a flexural strength of 515MPa.
Example 4
S1, performing wet ball milling and mixing on 500g of nano aluminum nitride powder (with the particle size of 50 nm), 30g of magnesium fluoride and absolute ethyl alcohol, wherein a grinding medium is high-purity zirconia balls, and drying and sieving to obtain mixed powder after ball milling and mixing uniformly;
s2, putting the mixed powder into a sintering furnace, and performing pre-pressing treatment under the pressure of 10MPa to obtain a pre-pressed body;
and S3, simultaneously applying dynamic pressure (the pressure is 50 +/-10 MPa and the frequency is 1 Hz) and ultrasonic waves (the frequency is 20 KHz) to the pre-pressing body, heating to 1600 ℃ at the heating rate of 20 ℃/min, and preserving heat for 4h to obtain the aluminum nitride ceramic.
The aluminum nitride ceramic prepared in example 4 has a density of 99.6%, a thermal conductivity of 110W/m.K, and a bending strength of 575MPa.
Example 5
S1, performing wet ball milling and mixing on 500g of nano aluminum nitride powder (with the particle size of 50 nm), 15g of yttrium fluoride, 15g of calcium fluoride and absolute ethyl alcohol, wherein a grinding medium is high-purity zirconia balls, and drying and sieving to obtain mixed powder after ball milling and mixing uniformly;
s2, placing the mixed powder into a sintering furnace, and performing pre-pressing treatment under the pressure of 10MPa to obtain a pre-pressed body;
and S3, simultaneously applying dynamic pressure (the pressure is 45 +/-10 MPa, the frequency is 2 Hz) and ultrasonic waves (the frequency is 20 KHz) to the pre-pressing body, heating to 1600 ℃ at the heating rate of 20 ℃/min, and preserving heat for 6 hours to obtain the aluminum nitride ceramic.
The aluminum nitride ceramic prepared in example 5 has a density of 99.7%, a thermal conductivity of 120W/m.K, and a bending strength of 610MPa.
Comparative example 1
S1, performing wet ball milling and mixing on 500g of nano aluminum nitride powder (with the particle size of 50 nm), 10g of yttrium fluoride, 10g of calcium fluoride, 10g of magnesium fluoride and absolute ethyl alcohol, wherein a grinding medium is high-purity zirconia balls, and drying and sieving to obtain mixed powder after ball milling and mixing uniformly;
s2, putting the mixed powder into a sintering furnace, and performing pre-pressing treatment under the pressure of 10MPa to obtain a pre-pressed body;
and S3, under the action of applying dynamic pressure (the pressure is 50 +/-10 MPa, the frequency is 2 Hz) to the pre-pressing body, heating to 1600 ℃ at the heating rate of 20 ℃/min, and preserving heat for 6h to obtain the aluminum nitride ceramic.
The aluminum nitride ceramic prepared in comparative example 1 had a density of 99.3%, a thermal conductivity of 95W/m.K, and a flexural strength of 490MPa.
Comparative example 2
S1, performing wet ball milling and mixing on 500g of nano aluminum nitride powder (with the particle size of 50 nm), 10g of yttrium fluoride, 10g of calcium fluoride, 10g of magnesium fluoride and absolute ethyl alcohol, wherein a grinding medium is high-purity zirconia balls, and drying and sieving to obtain mixed powder after ball milling and mixing uniformly;
s2, putting the mixed powder into a sintering furnace, and performing pre-pressing treatment under the pressure of 10MPa to obtain a pre-pressed body;
and S3, under the action of applying constant pressure (the pressure is 50 MPa) to the pre-pressing body, heating to 1600 ℃ at the heating rate of 20 ℃/min, and preserving heat for 6h to obtain the aluminum nitride ceramic.
The aluminum nitride ceramic prepared in comparative example 2 has a density of 98.4%, a thermal conductivity of 78W/m.K, and a bending strength of 390MPa.
Comparative example 3
S1, performing wet ball milling and mixing on 500g of nano aluminum nitride powder (with the particle size of 50 nm), 10g of yttrium fluoride, 10g of calcium fluoride, 10g of magnesium fluoride and absolute ethyl alcohol, wherein a grinding medium is high-purity zirconia balls, and drying and sieving to obtain mixed powder after ball milling and mixing uniformly;
s2, putting the mixed powder into a sintering furnace, and performing pre-pressing treatment under the pressure of 10MPa to obtain a pre-pressed body;
and S3, under the action of applying constant pressure (the pressure is 50 MPa) and ultrasonic waves (the frequency is 20 KHz) to the pre-pressing body, heating to 1600 ℃ at the heating rate of 20 ℃/min, and preserving heat for 6h to obtain the aluminum nitride ceramic.
The aluminum nitride ceramic prepared in comparative example 3 had a density of 98.8%, a thermal conductivity of 83W/m.K, and a flexural strength of 415MPa.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of high-density aluminum nitride ceramic is characterized by comprising the following steps:
s1, carrying out ball milling and mixing on nano aluminum nitride powder, a sintering aid and a solvent to obtain mixed powder;
s2, pre-pressing the mixed powder to obtain a pre-pressed body;
s3, sintering the pre-pressing body under the action of dynamic pressure and ultrasonic waves to obtain the aluminum nitride ceramic; applying the dynamic pressure in a thickness direction of the pre-compact; the ultrasonic waves are applied in a direction perpendicular to the thickness of the pre-compact.
2. The production method according to claim 1, wherein the mass ratio of the aluminum nitride nanopowder to the sintering aid is (90-98): 2-10.
3. The preparation method according to claim 1, wherein the sintering aid is one or more of yttrium fluoride, calcium fluoride and magnesium fluoride;
the solvent is absolute ethyl alcohol.
4. The method of claim 1, further comprising the steps of drying and sieving after the ball milling and mixing.
5. The production method according to claim 1, wherein the pressure of the preliminary press treatment is 5 to 20MPa.
6. The method of claim 1, wherein the dynamic pressure is in a range of 30 ± 5MPa to 50 ± 10MPa;
the frequency of the dynamic pressure is 1-5 Hz.
7. The method according to claim 1, wherein the ultrasonic wave has a frequency of 20KHz.
8. The method according to claim 1, wherein the sintering treatment is carried out at a temperature rise rate of 10 to 20 ℃/min to 1500 to 1600 ℃.
9. A high-density aluminum nitride ceramic, which is prepared by the preparation method of any one of claims 1 to 8.
10. The aluminum nitride ceramic of claim 9, wherein the aluminum nitride ceramic has a compactness of not less than 99.4%, a thermal conductivity of not less than 100W/m-K, and a bending strength of not less than 500MPa.
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2022
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