CN107353001B - Preparation method of metal-based ceramic material - Google Patents

Preparation method of metal-based ceramic material Download PDF

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CN107353001B
CN107353001B CN201710555855.4A CN201710555855A CN107353001B CN 107353001 B CN107353001 B CN 107353001B CN 201710555855 A CN201710555855 A CN 201710555855A CN 107353001 B CN107353001 B CN 107353001B
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刘洪喜
刘子峰
张晓明
胡建力
周荣
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Kunming University of Science and Technology
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Abstract

The invention discloses a preparation method of a metal-based ceramic material, which belongs to the technical field of preparation of metal-based ceramic materials4(ii) a The good bonding between the powders of the cermet materials obtained, FeNbO, is obtained from the test data4The ceramic reinforcing phase improves the bonding strength of the sintered material, reduces the dislocation expansion sensitivity, has higher density and reduced porosity, and can promote the industrial application of the material to a great extent.

Description

Preparation method of metal-based ceramic material
Technical Field
The invention belongs to the technical field of preparation of metal ceramic materials, and particularly relates to a preparation method of a metal-based ceramic material.
Background
With the continuous extension of the application field of materials, the metal-based ceramic materials are continuously applied in the material industry due to the characteristics of high temperature resistance and excellent acousto-optic electrical properties. The research on the metal-based ceramic material is receiving more and more attention, and a preparation technical system with multidisciplinary coexistence is gradually formed. When applied to the field of capacitors, the material is required to have high resistivity and large dielectric constant, and among them, rutile (TiO) is more frequently studied2) However, these ceramic materials have the disadvantages of single preparation process, poor economic performance and not wide application, and the problems of easy preparation and high cost need to be solved during application, so the present technicians are dedicated to develop better materials.
Based on the problems in the prior art, researchers begin to develop more excellent alloy materials, iron-based materials become one of the key points of the current research because of the excellent economic performance and the diversified structural composite forms, Chengdu Yi-State science and technology company limited also discloses a preparation method of a sintered Fe-Al-based alloy material, the prepared material has better high-temperature oxidation resistance, but the patent does not perfect and disclose the problem of porosity caused by the matching of a process scheme and powder, and the problem of the matching of the process or raw materials exists.
Disclosure of Invention
Aiming at the problems in the prior art, the invention adopts the organic binder to mix Fe-based powder for sintering, and prepares the metal-based composite ceramic material under the condition of improving the bonding strength.
The invention provides a preparation method of a metal-based ceramic material, which comprises the following specific steps:
(1) according to Fe54+x(Si3N4)12-x(BN)10Nb24The raw materials Fe and Si are weighed according to the stoichiometric ratio3N4BN and Nb powder, wherein x = 0-10, and fully grinding and uniformly mixing;
(2) adding a binder into the mixed powder obtained in the step (1) according to the mass ratio of the binder to the mixed powder of 1: 3-6, uniformly mixing, tabletting and presintering;
(3) and (3) cooling the product obtained after the pre-sintering in the step (2) to room temperature, adding Zr powder, grinding, adding an adhesive according to the mass ratio of the adhesive to the mixture of 1: 3-6, and uniformly mixing, tabletting and sintering to obtain the metal-based ceramic material, wherein the Zr powder accounts for 2.5-3.1% of the final mixture.
And (3) grinding for 0.5-2 h.
And (3) keeping the final pressure of the tabletting in the step (2) and the step (3) at 6-30 MPa for 1-5 min after 2-4 MPa is added from 0 MPa.
The shape of the tablet in the steps (2) and (3) is cylindrical, the diameter is 0.6-2 cm, and the thickness is 2.5-5 mm.
And (3) mixing the absolute ethyl alcohol and polyvinyl alcohol PVA L according to the mass ratio of 1: 3 to obtain the binder.
And (3) pre-sintering at 600-800 ℃ for 3-5 h in the air.
And (3) sintering at the temperature of 600-800 ℃ for 3-5 h, cooling to 400-500 ℃, preserving heat for 1-2 h, then heating to 1100-1250 ℃, preserving heat for 10-20 h, wherein the sintering atmosphere is air.
The invention has the beneficial effects that:
the process is convenient to realize, and special atmosphere protection is not needed during sintering; fe as a raw material is a low-cost metal, inThe dielectric ceramic FeNbO material has the advantages that materials are conveniently available during preparation of the dielectric ceramic, new elements are added during secondary sintering, a mode of temperature reduction and temperature rise is adopted in the secondary sintering process, the binder is mixed by absolute ethyl alcohol and PVA L, tabletting is more favorably prepared, the density of the material obtained by the method is higher, the reduction of the porosity can promote the industrial application of the material to a great extent, and the dielectric ceramic FeNbO material obtained by the method4Ingredients, which provide directions and experimental conditions for the preparation of the material; through a series of embodiments, under the same process, the thermal expansion coefficient and the density caused by different elements are different, particularly the density influence is caused, the density is reduced when the content of the Fe element is increased, the thermal expansion coefficient is increased, and the use of the ceramic material at the later stage is also influenced.
Drawings
FIG. 1 is a SEM-BSD picture of a metal-based ceramic material obtained in example 1 of the present invention;
FIG. 2 is a SEM-BSD picture of the metal-based ceramic material obtained in example 2 of the present invention;
FIG. 3 is a SEM-BSD picture of the metal-based ceramic material obtained in example 3 of the present invention.
Detailed Description
For the purpose of enhancing understanding of the present invention, the present invention will be further described with reference to specific examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
Example 1
A preparation method of a metal-based ceramic material comprises the following specific steps:
(1) according to Fe64(Si3N4)2(BN)10Nb24The raw materials Fe and Si are weighed by an electronic scale3N4BN and Nb powder are fully ground for 0.5h and mixed evenly;
(2) adding a binder into the mixed powder in the step (1) according to the mass ratio of the binder to the mixed powder of 1: 6, wherein the binder is formed by mixing absolute ethyl alcohol and polyvinyl alcohol PVA L according to the mass ratio of 1: 3, uniformly mixing, tabletting and presintering, the pressure of the tabletting is 20MPa, the pressure is maintained for 3min every time 4MPa is increased from 0, and finally the tabletting is cylindrical, the diameter is 2cm, the thickness is 2.5mm, the presintering condition is 800 ℃, the heat preservation time is 4h, and the atmosphere is air;
(3) cooling the product obtained after the pre-sintering in the step (2) to room temperature, adding Zr powder, grinding, wherein the Zr powder accounts for 3.1% of the final mixture by mass, adding an adhesive according to the mass ratio of the adhesive to the mixture of 1: 6, wherein the adhesive is formed by mixing absolute ethyl alcohol and polyvinyl alcohol PVA L according to the mass ratio of 1: 3, uniformly mixing, tabletting and sintering, the pressure of the tabletting is 20MPa, and the pressure is increased every 4MPa from 0 for 1min, and finally the tabletting is pressed into a cylinder shape with the diameter of 2cm and the thickness of 2.5mm, wherein the sintering condition is that the temperature is firstly increased to 800 ℃ and is kept for 4 hours under the air atmosphere, then the temperature is reduced to 400 ℃ and is kept for 2 hours, then the temperature is increased to 1100 ℃ and is kept for 20 hours, and the metal-based ceramic material is obtained after furnace cooling.
FIG. 1 is a SEM-BSD picture of the metal-based ceramic material obtained in this example, wherein the material is composed of white bone-like substances and gray substances, and Table 1 is the energy spectrum content of the white bone-like substances in the SEM-BSD picture of the metal-based ceramic material obtained in this example, wherein the white bone-like substances are FeNbO4Is a dielectric ceramic, and can be seen from SEM-BSD picture that the crack initiation generally staggers white substances, and the sample bonding is good, namely FeNbO4The ceramic reinforcing phase improves the bonding strength of the sintered material and reduces the dislocation propagation sensitivity, and the coefficient of thermal expansion of the metal-based ceramic material obtained in the embodiment is 5.8 × 10-6℃-1The degree of compactness was 95.2%.
TABLE 1
Figure 608314DEST_PATH_IMAGE001
。
Example 2
A preparation method of a metal-based ceramic material comprises the following specific steps:
(1) according to Fe60(Si3N4)6(BN)10Nb24The raw materials Fe and Fe are weighed by an electronic scale,Si3N4BN and Nb powder are fully ground for 2 hours and mixed evenly;
(2) adding a binder into the mixed powder in the step (1) according to the mass ratio of the binder to the mixed powder of 1: 5, wherein the binder is formed by mixing absolute ethyl alcohol and polyvinyl alcohol PVA L according to the mass ratio of 1: 3, uniformly mixing, tabletting and presintering, the pressure of the tabletting is 6MPa, the pressure is maintained for 5min every time 2MPa is increased from 0, and finally the tabletting is cylindrical, the diameter is 1cm, the thickness is 5mm, the presintering condition is 700 ℃, the heat preservation time is 5h, and the atmosphere is air;
(3) cooling the product obtained after the pre-sintering in the step (2) to room temperature, adding Zr powder, grinding, wherein the Zr powder accounts for 3% of the final mixture by mass, adding an adhesive according to the mass ratio of the adhesive to the mixture of 1: 4, wherein the adhesive is formed by mixing absolute ethyl alcohol and polyvinyl alcohol PVA L according to the mass ratio of 1: 3, uniformly mixing, tabletting and sintering, the pressure of the tabletting is 6MPa, and the pressure is maintained for 4min every 2MPa from 0, and finally the tabletting is cylindrical, the diameter is 1cm, the thickness is 5mm, the sintering condition is that the temperature is firstly increased to 700 ℃ and kept for 5 hours under the air atmosphere, then the temperature is reduced to 500 ℃ and kept for 1 hour, then the temperature is increased to 1250 ℃ and kept for 10 hours, and furnace cooling is carried out, so as to obtain the metal-based ceramic material.
FIG. 2 is a SEM-BSD picture of the cermet material obtained in this example, wherein the cermet material obtained in this example has less white bone and less dendrite formation, and Table 2 shows the energy spectrum content of the white bone in the SEM-BSD picture of the cermet material obtained in this example, wherein the dielectric ceramic FeNbO prepared in this example is shown in this figure4The coefficient of thermal expansion of the cermet material obtained in this example was found to be 5.4 × 10-6℃-1The degree of compactness was 96.5%.
TABLE 2
Figure 76467DEST_PATH_IMAGE002
。
Example 3
A preparation method of a metal-based ceramic material comprises the following specific steps:
(1) according to Fe54(Si3N4)12(BN)10Nb24The raw materials Fe and Si are weighed by an electronic scale3N4BN and Nb powder are fully ground for 1 hour and mixed evenly;
(2) adding a binder into the mixed powder in the step (1) according to the mass ratio of the binder to the mixed powder of 1: 3, wherein the binder is formed by mixing absolute ethyl alcohol and polyvinyl alcohol PVA L according to the mass ratio of 1: 3, uniformly mixing, tabletting and presintering, the pressure of the tabletting is 30MPa, the pressure is maintained for 1min every time 3MPa is increased from 0, and finally the tabletting is pressed into a cylinder shape with the diameter of 0.6cm and the thickness of 3mm, the presintering condition is that the temperature is 600 ℃, the heat preservation time is 3h, and the atmosphere is air;
(3) cooling the product obtained after the pre-sintering in the step (2) to room temperature, adding Zr powder, grinding, wherein the Zr powder accounts for 2.5% of the final mixture by mass, adding an adhesive according to the mass ratio of the adhesive to the mixture of 1: 3, wherein the adhesive is formed by mixing absolute ethyl alcohol and polyvinyl alcohol PVA L according to the mass ratio of 1: 3, uniformly mixing, tabletting and sintering, the pressure of the tabletting is 30MPa, the pressure is increased by 3MPa every time from 0 for 5min, the tabletting is finally pressed into a cylinder shape with the diameter of 0.6cm and the thickness of 3mm, the sintering condition is that the temperature is firstly increased to 600 ℃ and is kept for 3 hours in the air atmosphere, then the temperature is reduced to 450 ℃ and is kept for 1.5 hours, then the temperature is increased to 1200 ℃ and is kept for 15 hours, and the sintering is carried out in a furnace, and the metal-based ceramic.
FIG. 3 is a SEM-BSD picture of the cermet material obtained in the present example, wherein the cermet material obtained in the present example has less white bone substance, less dendrite formation and larger white bone structure, and Table 3 shows the energy spectrum content of the white bone substance in the SEM-BSD picture of the cermet material obtained in the present example, and the thermal expansion coefficient of the cermet material obtained in the present example is 4.2 × 10-6℃-1The density is 96.8 percent
TABLE 3
Figure 409359DEST_PATH_IMAGE003
。

Claims (6)

1. The preparation method of the metal-based ceramic material is characterized by comprising the following specific steps of:
(1) according to Fe54+x(Si3N4)12-x(BN)10Nb24The raw materials Fe and Si are weighed according to the stoichiometric ratio3N4BN and Nb powder, wherein x = 0-10, and fully grinding and uniformly mixing;
(2) adding a binder into the mixed powder obtained in the step (1) according to the mass ratio of the binder to the mixed powder of 1: 3-6, uniformly mixing, tabletting and presintering;
(3) and (3) cooling the product obtained after the pre-sintering in the step (2) to room temperature, adding Zr powder, grinding, wherein the Zr powder accounts for 2.5-3.1% of the final mixture by mass, adding an adhesive according to the mass ratio of the adhesive to the mixture of 1: 3-6, uniformly mixing, tabletting and sintering, wherein the sintering condition is that the temperature is 600-800 ℃, the heat preservation time is 3-5 h, the temperature is reduced to 400-500 ℃, the heat preservation time is 1-2 h, then the temperature is increased to 1100-1250 ℃, the heat preservation time is 10-20 h, and the sintering atmosphere is air, so that the metal-based ceramic material is obtained.
2. The method for preparing the metal-based ceramic material according to claim 1, wherein the grinding time in the step (1) and the step (3) is 0.5-2 h.
3. The method for preparing a metal-based ceramic material according to claim 1, wherein the final pressure of the tablet in the steps (2) and (3) is 6 to 30MPa, and the pressure is maintained for 1 to 5min for every 2 to 4MPa increase from 0 MPa.
4. The method for preparing a metal-based ceramic material according to claim 1, wherein the pellet of steps (2) and (3) has a cylindrical shape, a diameter of 0.6 to 2cm and a thickness of 2.5 to 5 mm.
5. The method for preparing the metal-based ceramic material according to claim 1, wherein the binder in the steps (2) and (3) is formed by mixing absolute ethyl alcohol and polyvinyl alcohol PVA L according to a mass ratio of 1: 3.
6. The preparation method of the metal-based ceramic material according to claim 1, wherein the pre-sintering condition in the step (2) is 600-800 ℃, the holding time is 3-5 h, and the atmosphere is air.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4150999A (en) * 1974-08-12 1979-04-24 Denki Kagaku Kogyo Kabushiki Kaisha Method for manufacture of ferrosilicon nitride
EP0160301B1 (en) * 1984-05-01 1989-07-12 Kabushiki Kaisha Toyota Chuo Kenkyusho Method of bonding ceramic article
CN1160273A (en) * 1997-02-26 1997-09-24 清华大学 Medium- and low-temp. sintered combined characteristic thermosensitive resistor material composition and preparing method
CN102775195A (en) * 2011-05-13 2012-11-14 比亚迪股份有限公司 Selective metallization method of surface of ceramic, and ceramic and its application
CN104046823A (en) * 2014-06-13 2014-09-17 上海和辉光电有限公司 Graded metal-ceramic composite and preparation method thereof
CN105060882A (en) * 2015-07-23 2015-11-18 罗美柏 Piezoceramic material and preparation method therefor

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4150999A (en) * 1974-08-12 1979-04-24 Denki Kagaku Kogyo Kabushiki Kaisha Method for manufacture of ferrosilicon nitride
EP0160301B1 (en) * 1984-05-01 1989-07-12 Kabushiki Kaisha Toyota Chuo Kenkyusho Method of bonding ceramic article
CN1160273A (en) * 1997-02-26 1997-09-24 清华大学 Medium- and low-temp. sintered combined characteristic thermosensitive resistor material composition and preparing method
CN102775195A (en) * 2011-05-13 2012-11-14 比亚迪股份有限公司 Selective metallization method of surface of ceramic, and ceramic and its application
CN104046823A (en) * 2014-06-13 2014-09-17 上海和辉光电有限公司 Graded metal-ceramic composite and preparation method thereof
CN105060882A (en) * 2015-07-23 2015-11-18 罗美柏 Piezoceramic material and preparation method therefor

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