CN116041069B - Ceramic material and preparation method thereof - Google Patents

Ceramic material and preparation method thereof Download PDF

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Publication number
CN116041069B
CN116041069B CN202211655234.0A CN202211655234A CN116041069B CN 116041069 B CN116041069 B CN 116041069B CN 202211655234 A CN202211655234 A CN 202211655234A CN 116041069 B CN116041069 B CN 116041069B
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sintering
ceramic material
aln
thermal conductivity
grinding
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CN116041069A (en
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杨治华
赵哲
周国相
贾德昌
周玉
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention belongs to the technical field of ceramics, and particularly relates to a ceramic material and a preparation method thereof. The ceramic material provided by the invention comprises the following raw materials: alN and a nitride selected from VN, tiN, zrN, crN, BN, si 3 N 4 At least 3 of (3); or AlN with an element selected from at least 3 of V, ti, zr, cr, ni, B, si; alternatively, alN and an oxide selected from VO 2 、TiO 2 、ZrO 2 、Cr 2 O 3 、B 2 O 3 、SiO 2 At least 3 of (3); or AlN, an oxide and an element, wherein the oxide and the element at least contain 3 different raw materials, the oxide is selected from at least 1 of the above oxides, and the element is selected from at least 1 of the above elements. The thermal conductivity of the prepared ceramic material is increased along with the temperature rise through the mutual doping of the powder, and the ceramic material has a positive thermal conductivity effect.

Description

Ceramic material and preparation method thereof
Technical Field
The invention belongs to the technical field of ceramics, and particularly relates to a ceramic material and a preparation method thereof.
Background
Ceramics are an indispensable material in human life and production, and along with the continuous development of social technology, ceramic materials are developed very rapidly, raw materials adopted by the ceramics are not only natural minerals or clay, but also a plurality of chemical materials which are manually purified and synthesized are listed as optional raw materials, and the optional raw materials comprise inorganic nonmetallic materials. The existing ceramic material becomes one of the most potential development materials after metal materials and high polymer materials, and has the advantages of high melting point, high thermal conductivity, high hardness, high wear resistance, oxidation resistance and the like, and has a wide application prospect.
The ceramic material has wide application in the fields of temperature control, heat dissipation and the like due to good heat conductivity, but the heat conductivity of the traditional ceramic material gradually decreases or tends to be stable along with the temperature rise, so that the high-temperature heat dissipation efficiency of the ceramic material is influenced, the application range of the ceramic material is greatly limited, and no research and report on the ceramic material with the positive temperature effect of the heat conductivity are available at present.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect that the thermal conductivity of the ceramic material gradually decreases or tends to be stable along with the temperature rise in the prior art, thereby providing a ceramic material with positive thermal conductivity and a preparation method thereof.
The invention provides a ceramic material, which comprises the following raw materials:
AlN and a nitride selected from VN, tiN, zrN, crN, BN, si 3 N 4 At least 3 of (3);
or AlN with an element selected from at least 3 of V, ti, zr, cr, ni, B, si;
alternatively, alN and an oxide selected from VO 2 、TiO 2 、ZrO 2 、Cr 2 O 3 、B 2 O 3 、SiO 2 At least 3 of (3);
alternatively, alN, an oxide and an element, the oxide and the element containing at least 3 different raw materials, the oxide being selected from VO 2 、TiO 2 、ZrO 2 、Cr 2 O 3 、B 2 O 3 、SiO 2 At least 1 element selected from V, ti, zr, cr, ni, B, si.
Optionally, the selected raw material is powder.
Preferably, when the starting material is selected from AlN and nitrides, the nitrides are selected from VN, tiN, zrN, crN, BN, si 3 N 4 At least 3 of (3), the mass ratio of AlN to nitride is (1-50): (50-99);
when the raw material is selected from AlN and simple substance, and the simple substance is selected from at least 3 of V, ti, zr, cr, ni, B, si, the mass ratio of AlN to simple substance is (1-50): (50-99);
when the raw material is selected from AlN and oxide, the oxide is selected from VO 2 、TiO 2 、ZrO 2 、Cr 2 O 3 、B 2 O 3 、SiO 2 At least 3 of (a) AlN and an oxide in a mass ratio of (1-50): (50-99);
when the raw materials are selected from AlN, oxides and simple substances, the oxides and simple substances at least contain 3 different raw materials, and the oxides are selected from VO 2 、TiO 2 、ZrO 2 、Cr 2 O 3 、B 2 O 3 、SiO 2 When the simple substance is selected from at least 1 of V, ti, zr, cr, ni, B, si, the mass ratio of the total mass of the oxide and the simple substance to AlN is (50-99): (1-50).
Preferably, the ceramic material comprises the following raw materials: alN, crN, tiN, BN and Si 3 N 4 AlN, crN, tiN, BN and Si 3 N 4 The mass ratio of (2) is 1: (0.5-2): (0.5-2): (0.5-2): (0.5-2).
Preferably, the ceramic material comprises the following raw materials: alN, cr, ti, zr, V, ni, B and Si, the mass ratio of AlN, cr, ti, zr, V, ni, B, si is 1: (0.5-2): (0.5-2): (0.5-1): (0.5-2): (0.5-2): (0.5-2): (0.5-2).
Preferably, the ceramic material comprises the following raw materials: alN, VO 2 、TiO 2 、ZrO 2 、Cr 2 O 3 、B 2 O 3 And SiO 2 The AlN, VO 2 、TiO 2 、ZrO 2 、Cr 2 O 3 、B 2 O 3 、SiO 2 The mass ratio of (2) is 1: (0.2-1): (0.2-1): (0.2-1): (0.2-1): (0.2-1): (0.2-1).
Preferably, the ceramic material comprises the following raw materials: alN, crN, tiN, zrN and BN, the mass ratio of AlN, crN, tiN, zrN, BN is 1: (0.5-2): (0.5-2): (0.5-2): (0.5-2).
Preferably, the ceramic material is a ceramic material with a positive temperature effect of thermal conductivity.
The invention provides a preparation method of the ceramic material, which comprises the following steps:
1) Weighing the raw materials according to the formula proportion, mixing and grinding the raw materials to obtain mixed powder;
2) And filling the mixed powder into a die for sintering to obtain the ceramic material.
Preferably, in the step 1), the grinding rotation speed is 20-1000r/min, the grinding time is 0.5-80h, and the grinding atmosphere is air, vacuum, nitrogen or argon;
the material of the die in the step 2) is selected from one of high-purity graphite, carbon-carbon composite material and diamond;
the sintering in the step 2) is air pressure sintering or hot press sintering.
Optionally, the grinding mode is ball milling, and the ball-to-material ratio is (2-50): 1.
Optionally, the ball milling tank and the ball mill can be made of agate, silicon nitride, sintered corundum, zirconia, chrome steel, nylon and other materials; the ball milling lubricant is absolute ethyl alcohol.
Preferably, the sintering in the step 2) is hot-press sintering, the sintering temperature is 800-2000 ℃, the sintering pressure is 0.1-60MPa, and the heat preservation time is 0.1-12h;
the temperature rising rate of the sintering is 0.5-25 ℃/min;
the sintering atmosphere of the sintering is air, vacuum, nitrogen or argon;
the step 2) is further comprised of pre-pressing the mixed powder loaded into the mold before the sintering step. Optionally, the pre-pressing pressure is 0.1-40MPa, and the pre-pressing mode is selected from but not limited to hydraulic press.
Optionally, naturally cooling to room temperature after sintering.
The technical scheme of the invention has the following advantages:
(1) The ceramic material provided by the invention comprises the following raw materials: alN and nitride, the nitrogenThe compound is selected from VN, tiN, zrN, crN, BN, si 3 N 4 At least 3 of (3); or AlN with an element selected from at least 3 of V, ti, zr, cr, ni, B, si; alternatively, alN and an oxide selected from VO 2 、TiO 2 、ZrO 2 、Cr 2 O 3 、B 2 O 3 、SiO 2 At least 3 of (3); alternatively, alN, an oxide and an element, the oxide and the element containing at least 3 different raw materials, the oxide being selected from VO 2 、TiO 2 、ZrO 2 、Cr 2 O 3 、B 2 O 3 、SiO 2 At least 1 element selected from V, ti, zr, cr, ni, B, si. According to the invention, alN ceramic with excellent heat conduction characteristics is taken as a basis, and the specific powder is doped with each other to change the phonon heat transfer process of AlN by matching with lattice and solid solubility of AlN, so that the prepared ceramic material has heat conductivity which is increased along with the increase of temperature, has a positive heat effect of heat conductivity, and is beneficial to realizing independent regulation and control of the heat conduction properties of the ceramic material in different environments.
(2) The ceramic material provided by the invention comprises the following raw materials: alN, crN, tiN, zrN and BN, the mass ratio of AlN, crN, tiN, zrN, BN is 1: (0.5-2): (0.5-2): (0.5-1): (0.5-2). The ceramic material obtained by the specific powder and the specific proportion has the positive temperature effect of heat conductivity, and the heat conductivity of the ceramic material is increased along with the temperature rise.
(3) The preparation method of the ceramic material provided by the invention comprises the following steps: 1) Weighing the raw materials according to the formula proportion, mixing and grinding the raw materials to obtain mixed powder; 2) And filling the mixed powder into a die for sintering to obtain the ceramic material. The ceramic block is prepared by mechanical mixing and solid-phase reaction sintering, the preparation process is simple and environment-friendly, and the ceramic material with the positive temperature effect of thermal conductivity is finally obtained.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph of thermal conductivity versus temperature for example 1 of the present invention;
FIG. 2 is a graph of thermal conductivity versus temperature for comparative example 1 of the present invention.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Example 1
The embodiment provides a preparation method of a ceramic material, which comprises the following steps:
1) Weighing AlN, crN, tiN, zrN, BN powder according to the mass ratio of 1:1:1:1, mixing, ball milling by using a planetary ball mill, wherein the grinding balls are silicon nitride balls, the ball-material ratio is 10:1, the lubricant is absolute ethyl alcohol, the grinding speed is 300r/min, the ball milling time is 24 hours, and the grinding atmosphere is air, so that mixed powder is obtained.
2) Loading the mixed powder into a graphite die for hot-pressing sintering, pre-pressing by using a hydraulic press before sintering, wherein the pressure is 10MPa, the sintering heating rate is 20 ℃/min, the sintering temperature is 1800 ℃, the sintering pressure is 30MPa, the heat preservation time is 1h, and the sintering atmosphere is nitrogen; and naturally cooling to room temperature after sintering to obtain the ceramic block.
The prepared ceramic was tested for thermal conductivity using a German relaxation-resistant LFA467 laser thermal conductivity meter, and the resulting thermal conductivity profile as a function of temperature was shown in FIG. 1. The thermal conductivity of the ceramic can reach 5.8W/(m.K) at-60 ℃, 13.9W/(m.K) at 700 ℃, and the thermal conductivity can be changed by more than 2 times within the range of-60 ℃ to 700 ℃.
Example 2
The embodiment provides a preparation method of a ceramic material, which comprises the following steps:
1) AlN, crN, tiN, BN, si is weighed according to the mass ratio of 1:1:1:1:1 3 N 4 Mixing the powder, ball milling the powder by using a planetary ball mill, wherein the grinding balls are silicon nitride balls, the ball-material ratio is 50:1, the lubricant is absolute ethyl alcohol, the grinding speed is 1000r/min, the ball milling time is 0.5h, and the grinding atmosphere is air, so as to obtain the mixed powder.
2) Loading the mixed powder into a graphite die for hot-pressing sintering, pre-pressing by using a hydraulic press before sintering, wherein the pressure is 20MPa, the sintering heating rate is 25 ℃/min, the sintering temperature is 800 ℃, the sintering pressure is 60MPa, the heat preservation time is 12h, and the sintering atmosphere is nitrogen; and naturally cooling to room temperature after sintering to obtain the ceramic block.
Example 3
The embodiment provides a preparation method of a ceramic material, which comprises the following steps:
1) Weighing AlN, cr, ti, zr, V, ni, B, si powder according to the mass ratio of 1:1:1:1:1:1:1, mixing, ball milling by using a planetary ball mill, wherein grinding balls are silicon nitride balls, the ball-material ratio is 10:1, the lubricant is absolute ethyl alcohol, the grinding rotating speed is 200r/min, the ball milling time is 80h, and the grinding atmosphere is air, so that mixed powder is obtained.
2) Loading the mixed powder into a graphite die for hot-pressing sintering, pre-pressing by using a hydraulic press before sintering, wherein the pressure is 30MPa, the sintering heating rate is 0.5 ℃/min, the sintering temperature is 2000 ℃, the sintering pressure is 40MPa, the heat preservation time is 0.5h, and the sintering atmosphere is nitrogen; and naturally cooling to room temperature after sintering to obtain the ceramic block.
Example 4
The embodiment provides a preparation method of a ceramic material, which comprises the following steps:
1) AlN and VO are weighed according to the mass ratio of 1:1:1:1:1:1 2 、TiO 2 、ZrO 2 、Cr 2 O 3 、B 2 O 3 、SiO 2 Mixing the powder, ball milling the powder by using a planetary ball mill, wherein the grinding balls are silicon nitride balls, the ball-material ratio is 20:1, the lubricant is absolute ethyl alcohol, the grinding speed is 800r/min, the ball milling time is 24h, and the grinding atmosphere is nitrogen, so that the mixed powder is obtained.
2) Loading the mixed powder into a graphite die for hot-pressing sintering, pre-pressing by using a hydraulic press before sintering, wherein the pressure is 40MPa, the sintering heating rate is 10 ℃/min, the sintering temperature is 1200 ℃, the sintering pressure is 10MPa, the heat preservation time is 6h, and the sintering atmosphere is argon; and naturally cooling to room temperature after sintering to obtain the ceramic block.
Comparative example 1
This comparative example provides a ceramic material comprising AlN and Y 2 O 3 Composition, wherein Y 2 O 3 The addition amounts of (a) are respectively 0%, 1%, 3%, 5% and 7%, and the thermal conductivity of the ceramic material is tested, so that the curve of the thermal conductivity changing with temperature is shown in figure 2.
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 invention.

Claims (1)

1. The preparation method of the ceramic material with the positive thermal conductivity and temperature effect is characterized by comprising the following steps of:
1) Weighing AlN, crN, tiN, zrN, BN powder according to the mass ratio of 1:1:1:1, mixing, ball milling by using a planetary ball mill, wherein the grinding balls are silicon nitride balls, the ball-material ratio is 10:1, the lubricant is absolute ethyl alcohol, the grinding speed is 300r/min, the ball milling time is 24 hours, and the grinding atmosphere is air, so that mixed powder is obtained;
2) Loading the mixed powder into a graphite die for hot-pressing sintering, pre-pressing by using a hydraulic press before sintering, wherein the pressure is 10MPa, the sintering heating rate is 20 ℃/min, the sintering temperature is 1800 ℃, the sintering pressure is 30MPa, the heat preservation time is 1h, and the sintering atmosphere is nitrogen; and after sintering, naturally cooling to room temperature to obtain the ceramic material with positive thermal conductivity and temperature effect.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105503199A (en) * 2015-12-30 2016-04-20 山东大学 High-heat conductivity silicon nitride-aluminum nitride composite material and preparation method thereof

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EP3042885B1 (en) * 2013-09-02 2022-06-01 NGK Insulators, Ltd. A method comprising using a ceramic material as a thermal switch

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