CN113880591A - Silicon nitride-based ceramic body and method for in-situ self-generating zirconium nitride coating on surface of silicon nitride-based ceramic - Google Patents

Silicon nitride-based ceramic body and method for in-situ self-generating zirconium nitride coating on surface of silicon nitride-based ceramic Download PDF

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CN113880591A
CN113880591A CN202111262540.3A CN202111262540A CN113880591A CN 113880591 A CN113880591 A CN 113880591A CN 202111262540 A CN202111262540 A CN 202111262540A CN 113880591 A CN113880591 A CN 113880591A
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sintering
silicon nitride
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王曲
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Shenzhen Chenyu Technology Co ltd
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Abstract

The invention discloses a silicon nitride-based ceramic body which has simple process and low cost and is more beneficial to practical production and application, and a method for in-situ self-generating a zirconium nitride coating on the surface of the silicon nitride-based ceramic body. The technical scheme adopted by the invention is as follows: a method for in-situ self-generating a zirconium nitride coating on the surface of silicon nitride-based ceramic comprises the following steps: (1) proportioning raw materials, including: 60-85wt% of silicon nitride, 5-30wt% of zirconium dioxide and 5-20wt% of sintering aid; (2) uniformly mixing the raw materials prepared in the step (1); (3) granulating the mixture obtained in the step (2); (4) carrying out compression molding on the granulated material obtained in the step (3); (5) and (4) sintering the molding material obtained in the step (4) in a graphite porcelain boat, wherein the sintering process is carried out in an inert atmosphere environment.

Description

Silicon nitride-based ceramic body and method for in-situ self-generating zirconium nitride coating on surface of silicon nitride-based ceramic
Technical Field
The invention relates to the technical field of preparation of inorganic non-metallic materials, in particular to a silicon nitride-based ceramic body and a method for in-situ self-generating a zirconium nitride coating on the surface of the silicon nitride-based ceramic body.
Background
The metal ceramic heating body mainly takes an alumina casting blank and an alumina rod core as matrixes, and the matrixes are screen-printed with screensThe circuit is prepared. Because of the low thermal conductivity of alumina, the heat-generating efficiency of the heating body is greatly influenced. Silicon nitride (Si)3N4) The ceramic body has good mechanical properties at normal temperature and high temperature, thermal shock resistance, oxidation resistance, wear resistance, corrosion resistance and heat conductivity, has special use value in the working environment of high temperature, high speed and strong corrosive medium, and is considered as the high-temperature structural ceramic with the most development potential. In recent years, research and development have been competitively conducted at home and abroad, and the application range of the ceramic heating element has been expanded.
Disclosure of Invention
The invention mainly aims to provide a silicon nitride-based ceramic body which has simple process and low cost and is more beneficial to practical production and application and a method for in-situ self-generating a zirconium nitride coating on the surface of the silicon nitride-based ceramic.
In order to achieve the above purpose, the invention adopts the following technical scheme.
The invention discloses a method for in-situ self-generating a zirconium nitride coating on the surface of silicon nitride-based ceramic, which comprises the following steps:
(1) proportioning raw materials, including: 60-85wt% of silicon nitride, 5-30wt% of zirconium dioxide and 5-20wt% of sintering aid;
(2) uniformly mixing the raw materials prepared in the step (1);
(3) granulating the mixture obtained in the step (2);
(4) carrying out compression molding on the granulated material obtained in the step (3); and
(5) and (4) sintering the molding material obtained in the step (4) in a graphite porcelain boat, wherein the sintering process is carried out in an inert atmosphere environment.
Further, the sintering aid is one or two of magnesium oxide and lithium fluoride.
The mixing in the step (2) is ball milling in a ball mill; the condition parameters of ball milling are as follows: the ball milling rotation speed is 300-.
And (3) granulating the mixture by using polyvinyl alcohol as a binder, and ageing for 24 hours after granulating.
The molding condition parameters in the step (4) include: the molding pressure is 50-200MPa, and the molding pressure is kept for 10-60 s.
The inert atmosphere is a nitrogen atmosphere.
The sintering condition parameters are as follows: gradually increasing the sintering temperature from room temperature to a target sintering temperature of 1500-1700 ℃, wherein the heating rate is 1-10 ℃/min, and when the target sintering temperature is reached, keeping the target sintering temperature for 1-5 h.
The sintering condition parameters are as follows: gradually increasing the sintering temperature from room temperature to a target sintering temperature of 1600-1650 ℃, wherein the heating rate is 2-8 ℃/min, and when the target sintering temperature is reached, keeping the target sintering temperature for 2-5 h.
The sintering condition parameters comprise: gradually increasing the sintering temperature from room temperature to a target sintering temperature of 1600-1620 ℃, wherein the temperature increase rate is 4-6 ℃/min, and when the target sintering temperature is reached, keeping the target sintering temperature for 3-4 h.
The invention also discloses a silicon nitride-based ceramic body, the surface of which is provided with a zirconium nitride coating; the composition mainly comprises the following components in percentage by weight: 60-85wt% of silicon nitride, 5-30wt% of zirconium dioxide and 5-20wt% of sintering aid.
Compared with the prior art, its beneficial effect is: because the zirconium nitride (Zr-N) has the characteristics of good electric conduction, high temperature resistance, corrosion resistance and wear resistance, the zirconium nitride coating is self-generated on the surface of the silicon nitride-based ceramic substrate in situ, so that the metal ceramic heating body is prepared in one step, the production process can be greatly simplified, and the production period can be shortened. Therefore, the technical scheme can solve the practical problems of complex preparation process and long production period of the metal ceramic heating body, thereby reducing the production cost and being more beneficial to practical production.
In addition, the zirconium nitride layer formed on the surface of the silicon nitride-based ceramic substrate in situ is bonded with the substrate by chemical bonds, so that the bonded body has high strength and is not easy to separate.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings required to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic flow chart of a method for in-situ self-generation of a zirconium nitride coating on a silicon nitride-based ceramic surface according to an embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the embodiments and the accompanying drawings. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Furthermore, the endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein. The technical features mentioned in the different embodiments of the invention described below can be combined with each other as long as they do not conflict with each other.
The method for in-situ self-generating zirconium nitride coating on the surface of silicon nitride-based ceramic is a flow chart of the method for in-situ self-generating zirconium nitride coating on the surface of silicon nitride-based ceramic provided by the preferred embodiment of the invention. The preferred embodiment discloses:
example 1
A silicon nitride-based ceramic body, the surface of which is self-generated with a zirconium nitride coating in situ; the composition mainly comprises the following components in percentage by weight: 80wt% of silicon nitride, 10wt% of zirconium dioxide and 10wt% of sintering aid. The sintering aid is magnesium oxide (MgO) or lithium fluoride (LiF).
The preparation method is shown in figure 1:
extracting raw materials in step (1): 24.0g of silicon nitride powder, 3.0g of zirconium dioxide powder and 3.0g of sintering aid were weighed. The sintering aid is selected from magnesia (MgO) powder and is used for reducing the sintering temperature of the ceramic.
Ball milling: the prepared raw materials are mixed and homogenized by an XGB2 planetary ball mill. Wherein the ball milling speed is 500r/min, and the ball milling time is 3 h; ethanol is used as a ball milling medium. Wherein the ball mill: raw materials: the mass ratio of ethanol is 4: 2: 1.
and (3) granulating and staling: and (3) granulating the uniformly mixed raw material powder by taking PVA (polyvinyl alcohol) with the concentration of 5wt% as a binder, and then ageing for 24 hours.
And (4) forming: the granulated material is subjected to compression molding (molding pressure is 120MPa, and pressure is maintained for 30 s) to obtain a ceramic green body to be sintered.
And (5) normal pressure sintering: placing the ceramic green body obtained in the step (4) into a graphite porcelain boat, and then placing the graphite porcelain boat into a tube furnace for sintering. The sintering process is carried out in a tubular furnace, the sintering atmosphere is nitrogen, the target sintering temperature is 1600 ℃, the heating rate is 6 ℃/min, and the target sintering temperature is kept for 4h after the target sintering temperature is reached.
The silicon nitride-based ceramic body sample prepared by the steps is tested, a yellow, uniform and bright coating is formed on the surface of the prepared sample, and XRD (X-ray diffraction) tests show that the coating is zirconium nitride and the resistance of the sample is 0.82 omega.
Example 2
A silicon nitride-based ceramic body, the surface of which is self-generated with a zirconium nitride coating in situ; the composition mainly comprises the following components in percentage by weight: 75wt% of silicon nitride, 15wt% of zirconium dioxide and 10wt% of sintering aid. The sintering aid is magnesium oxide (MgO) or lithium fluoride (LiF) and is used for reducing the sintering temperature of the ceramic.
The preparation method comprises the following steps:
1) extracting raw materials: 22.5g of silicon nitride powder, 4.5g of zirconium dioxide powder and 3.0g of sintering aid are weighed, wherein the sintering aid is lithium fluoride (LiF).
Ball milling: the prepared raw materials are mixed and homogenized by an XGB2 planetary ball mill. Wherein the ball milling speed is 500r/min, and the ball milling time is 3 h; ethanol is used as a ball milling medium. Wherein the ball mill: raw materials: the mass ratio of ethanol is 4: 2: 1.
and (3) granulating and staling: and (3) granulating the uniformly mixed raw material powder by taking PVA (polyvinyl alcohol) with the concentration of 5wt% as a binder, and then ageing for 24 hours.
And (4) forming: the granulated material is subjected to compression molding (molding pressure is 200MPa, and pressure is maintained for 10 s) to obtain a ceramic green body to be sintered.
And (5) normal pressure sintering: and (4) placing the ceramic green body obtained in the step (4) into a graphite porcelain boat, and then placing the graphite porcelain boat into a tube furnace for sintering. The sintering process is carried out in a tubular furnace, the sintering atmosphere is nitrogen, the target sintering temperature is 1600 ℃, the heating rate is 2 ℃/min, and the target sintering temperature is kept for 2h after the target sintering temperature is reached.
The silicon nitride-based ceramic body sample prepared by the steps is tested, a yellow, uniform and bright coating is generated on the surface of the prepared sample, XRD tests show that the coating is zirconium nitride, and the resistance of the sample is 0.74 omega.
Example 3
A silicon nitride-based ceramic body, the surface of which is self-generated with a zirconium nitride coating in situ; the composition mainly comprises the following components in percentage by weight: 70wt% of silicon nitride, 15wt% of zirconium dioxide and 15wt% of sintering aid. The sintering aid is a mixture of magnesium oxide and lithium fluoride and is used for reducing the sintering temperature of the ceramic.
The preparation method comprises the following steps:
extracting raw materials in step (1): 21g of silicon nitride powder, 4.5g of zirconium dioxide powder and 4.5g of sintering aid were weighed. The sintering aid is a mixture of magnesium oxide and lithium fluoride.
Ball milling: the prepared raw materials are mixed and homogenized by an XGB2 planetary ball mill. Wherein the ball milling speed is 500r/min, and the ball milling time is 4 h; ethanol is used as a ball milling medium. Wherein the ball mill: raw materials: the mass ratio of ethanol is 4: 2: 1.
and (3) granulating and staling: and (3) granulating the uniformly mixed raw material powder by taking PVA (polyvinyl alcohol) with the concentration of 5wt% as a binder, and then ageing for 24 hours.
And (4) forming: the granulated material is subjected to compression molding (molding pressure is 150MPa, and pressure is maintained for 25 s) to obtain a ceramic green body to be sintered.
And (5) normal pressure sintering: and (4) placing the ceramic green body obtained in the step (4) into a graphite porcelain boat, and then placing the graphite porcelain boat into a tube furnace for sintering. The sintering process is carried out in a tubular furnace, the sintering atmosphere is nitrogen, the target sintering temperature is 1650 ℃, the heating rate is 8 ℃/min, and the target sintering temperature is kept for 5 hours after the target sintering temperature is reached.
The silicon nitride-based ceramic body sample prepared by the steps is tested, a yellow, uniform and bright coating is generated on the surface of the prepared sample, XRD tests show that the coating is zirconium nitride, and the resistance of the sample is 0.86 omega.
Example 4
A silicon nitride-based ceramic body, the surface of which is self-generated with a zirconium nitride coating in situ; the composition mainly comprises the following components in percentage by weight: 65wt% of silicon nitride, 20wt% of zirconium dioxide and 15wt% of sintering aid. The sintering aid is magnesia powder and is used for reducing the sintering temperature of the ceramic.
The preparation method comprises the following steps:
extracting raw materials in step (1): 19.5g of silicon nitride powder, 6.0g of zirconium dioxide powder and 4.5g of sintering aid were weighed. The sintering aid is magnesium oxide powder.
Ball milling: the prepared raw materials are mixed and homogenized by an XGB2 planetary ball mill. Wherein the ball milling speed is 300r/min, and the ball milling time is 12 h; ethanol is used as a ball milling medium. Wherein the ball mill: raw materials: the mass ratio of ethanol is 4: 2: 1.
and (3) granulating and staling: and (3) granulating the uniformly mixed raw material powder by taking PVA (polyvinyl alcohol) with the concentration of 5wt% as a binder, and then ageing for 24 hours.
And (4) forming: the granulated material was press-molded (molding pressure 100MPa, holding pressure 40 s) to obtain a ceramic green compact.
And (5) normal pressure sintering: and (4) placing the ceramic green body obtained in the step (4) into a graphite porcelain boat, and then placing the graphite porcelain boat into a tube furnace for sintering. The sintering process is carried out in a tubular furnace, the sintering atmosphere is nitrogen, the target sintering temperature is 1650 ℃, the heating rate is 1 ℃/min, and the target sintering temperature is kept for 1h after reaching the target sintering temperature.
The silicon nitride-based ceramic body sample prepared by the steps is tested, a yellow, uniform and bright coating is generated on the surface of the prepared sample, XRD tests show that the coating is zirconium nitride, and the resistance of the sample is 0.80 omega.
Example 5
A silicon nitride-based ceramic body, the surface of which is self-generated with a zirconium nitride coating in situ; the composition mainly comprises the following components in percentage by weight: 60wt% of silicon nitride, 20wt% of zirconium dioxide and 20wt% of sintering aid. The sintering aid is lithium fluoride.
The preparation method comprises the following steps:
extracting raw materials in step (1): 18.0g of silicon nitride powder, 6g of zirconium dioxide powder and 6g of sintering aid were weighed. The sintering aid is lithium fluoride.
Ball milling: the prepared raw materials are mixed and homogenized by an XGB2 planetary ball mill. Wherein the ball milling speed is 400r/min, and the ball milling time is 6 h; ethanol is used as a ball milling medium. Wherein the ball mill: raw materials: the mass ratio of ethanol is 4: 2: 1.
and (3) granulating and staling: and (3) granulating the uniformly mixed raw material powder by taking PVA (polyvinyl alcohol) with the concentration of 5wt% as a binder, and then ageing for 24 hours.
And (4) forming: the granulated material was press-molded (molding pressure 50MPa, holding pressure 60 s) to obtain a ceramic green compact.
And (5) normal pressure sintering: and (4) placing the ceramic green body obtained in the step (4) into a graphite porcelain boat, and then placing the graphite porcelain boat into a tube furnace for sintering. The sintering process is carried out in a tubular furnace, the sintering atmosphere is nitrogen, the target sintering temperature is 1620 ℃, the heating rate is 4 ℃/min, and the target sintering temperature is kept for 3h after the target sintering temperature is reached.
The silicon nitride-based ceramic body sample prepared by the steps is tested, a yellow, uniform and bright coating is generated on the surface of the prepared sample, XRD tests show that the coating is zirconium nitride, and the resistance of the sample is 0.82 omega.
Example 6
A silicon nitride-based ceramic body, the surface of which is self-generated with a zirconium nitride coating in situ; the composition mainly comprises the following components in percentage by weight: 85wt% of silicon nitride, 10wt% of zirconium dioxide and 5wt% of sintering aid. The sintering aid is magnesium oxide.
The preparation method comprises the following steps:
extracting raw materials in step (1): 25.5g of silicon nitride powder, 3g of zirconium dioxide powder and 1.5g of sintering aid were weighed. The sintering aid is magnesium oxide.
Ball milling: the prepared raw materials are mixed and homogenized by an XGB2 planetary ball mill. Wherein the ball milling speed is 500r/min, and the ball milling time is 3 h; ethanol is used as a ball milling medium. Wherein the ball mill: raw materials: the mass ratio of ethanol is 4: 2: 1.
and (3) granulating and staling: and (3) granulating the uniformly mixed raw material powder by taking PVA (polyvinyl alcohol) with the concentration of 5wt% as a binder, and then ageing for 24 hours.
And (4) forming: the granulated material is subjected to compression molding (molding pressure is 120MPa, and pressure is maintained for 30 s) to obtain a ceramic green body to be sintered.
And (5) normal pressure sintering: and (4) placing the ceramic green body obtained in the step (4) into a graphite porcelain boat, and then placing the graphite porcelain boat into a tube furnace for sintering. The sintering process is carried out in a tubular furnace, the sintering atmosphere is nitrogen, the target sintering temperature is 1700 ℃, the heating rate is 5 ℃/min, and the target sintering temperature is kept for 3h after the target sintering temperature is reached.
The silicon nitride-based ceramic body sample prepared by the steps is tested, a yellow, uniform and bright coating is generated on the surface of the prepared sample, XRD tests show that the coating is zirconium nitride, and the resistance of the sample is 0.78 omega.
Example 7
A silicon nitride-based ceramic body, the surface of which is self-generated with a zirconium nitride coating in situ; the composition mainly comprises the following components in percentage by weight: 65wt% of silicon nitride, 30wt% of zirconium dioxide and 5wt% of sintering aid. The sintering aid is magnesium oxide.
The preparation method comprises the following steps:
extracting raw materials in step (1): 19.5g of silicon nitride powder, 9g of zirconium dioxide powder and 1.5g of sintering aid were weighed. The sintering aid is magnesium oxide.
Ball milling: the prepared raw materials are mixed and homogenized by an XGB2 planetary ball mill. Wherein the ball milling speed is 500r/min, and the ball milling time is 3 h; ethanol is used as a ball milling medium. Wherein the ball mill: raw materials: the mass ratio of ethanol is 4: 2: 1.
and (3) granulating and staling: and (3) granulating the uniformly mixed raw material powder by taking PVA (polyvinyl alcohol) with the concentration of 5wt% as a binder, and then ageing for 24 hours.
And (4) forming: the granulated material is subjected to compression molding (molding pressure is 120MPa, and pressure is maintained for 30 s) to obtain a ceramic green body to be sintered.
And (5) normal pressure sintering: placing the ceramic green body obtained in the step (4) into a graphite porcelain boat, and then placing the graphite porcelain boat into a tube furnace for sintering. The sintering process is carried out in a tubular furnace, the sintering atmosphere is nitrogen, the target sintering temperature is 1500 ℃, the heating rate is 10 ℃/min, and the target sintering temperature is kept for 5 hours after the target sintering temperature is reached.
The silicon nitride-based ceramic body sample prepared by the steps is tested, a yellow, uniform and bright coating is generated on the surface of the prepared sample, XRD tests show that the coating is zirconium nitride, and the resistance of the sample is 0.80 omega.
Example 8
A silicon nitride-based ceramic body, the surface of which is self-generated with a zirconium nitride coating in situ; the composition mainly comprises the following components in percentage by weight: 75wt% of silicon nitride, 5wt% of zirconium dioxide and 20wt% of sintering aid. The sintering aid is magnesium oxide.
The preparation method comprises the following steps:
extracting raw materials in step (1): 22.5g of silicon nitride powder, 1.5g of zirconium dioxide powder and 6.0g of sintering aid were weighed. The sintering aid is magnesium oxide.
Ball milling: mixing and homogenizing the prepared raw materials by adopting an XGB2 planetary ball mill, wherein the ball milling speed is 600r/min, and the ball milling time is 3 hours; ethanol is used as a ball milling medium. Wherein, the ball mill: raw materials: the mass ratio of ethanol is 4: 2: 1.
and (3) granulating and staling: and (3) granulating the uniformly mixed raw material powder by taking PVA (polyvinyl alcohol) with the concentration of 5wt% as a binder, and then ageing for 24 hours.
And (4) forming: the granulated material is subjected to compression molding (molding pressure is 120MPa, and pressure is maintained for 30 s) to obtain a ceramic green body to be sintered.
And (5) normal pressure sintering: placing the ceramic green body obtained in the step (4) into a graphite porcelain boat, and then placing the graphite porcelain boat into a tube furnace for sintering. The sintering process is carried out in a tubular furnace, the sintering atmosphere is nitrogen, the target sintering temperature is 1550 ℃, the heating rate is 4 ℃/min, and the target sintering temperature is kept for 2h after the target sintering temperature is reached.
The silicon nitride-based ceramic body sample prepared by the steps is tested, a yellow, uniform and bright coating is generated on the surface of the prepared sample, XRD tests show that the coating is zirconium nitride, and the resistance of the sample is 1.04 omega.
In the above embodiment, the sintering atmosphere in step (5) may be changed from nitrogen to argon.
Because the zirconium nitride (Zr-N) has the characteristics of good electric conduction, high temperature resistance, corrosion resistance and wear resistance, the zirconium nitride coating is self-generated on the surface of the silicon nitride-based ceramic substrate in situ, so that the metal ceramic heating body is prepared in one step, the production process can be greatly simplified, and the production period can be shortened. Therefore, the technical scheme can solve the practical problems of complex preparation process and long production period of the metal ceramic heating body, thereby reducing the production cost and being more beneficial to practical production. In addition, the zirconium nitride layer formed on the surface of the silicon nitride-based ceramic substrate in situ is bonded with the substrate by chemical bonds, so that the bonded body has high strength and is not easy to separate.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.

Claims (10)

1. A method for in-situ self-generating a zirconium nitride coating on the surface of silicon nitride-based ceramic comprises the following steps:
(1) proportioning raw materials, including: 60-85wt% of silicon nitride, 5-30wt% of zirconium dioxide and 5-20wt% of sintering aid;
(2) uniformly mixing the raw materials prepared in the step (1);
(3) granulating the mixture obtained in the step (2);
(4) carrying out compression molding on the granulated material obtained in the step (3); and
(5) and (4) sintering the molding material obtained in the step (4) in a graphite porcelain boat, wherein the sintering process is carried out in an inert atmosphere environment.
2. The method of claim 1, wherein the sintering aid is selected from one or both of magnesium oxide and lithium fluoride.
3. The method of claim 1, wherein the mixing in step (2) is ball milling in a ball mill; the condition parameters of ball milling are as follows: the ball milling rotation speed is 300-.
4. The method according to claim 1, wherein the granulating in step (3) is carried out by granulating the mixture with polyvinyl alcohol as a binder, and aging for 24h after granulating.
5. The method according to claim 1, wherein the condition parameters of the forming in step (4) include: the molding pressure is 50-200MPa, and the molding pressure is kept for 10-60 s.
6. The method of claim 1, wherein the inert atmosphere is a nitrogen atmosphere.
7. The method according to any one of claims 1 to 6, characterized in that the sintering condition parameters are: gradually increasing the sintering temperature from room temperature to a target sintering temperature of 1500-1700 ℃, wherein the heating rate is 1-10 ℃/min, and when the target sintering temperature is reached, keeping the target sintering temperature for 1-5 h.
8. The method according to claim 7, characterized in that the sintering condition parameters are: gradually increasing the sintering temperature from room temperature to a target sintering temperature of 1600-1650 ℃, wherein the heating rate is 2-8 ℃/min, and when the target sintering temperature is reached, keeping the target sintering temperature for 2-5 h.
9. The method according to claim 8, wherein the sintering condition parameters comprise: gradually increasing the sintering temperature from room temperature to a target sintering temperature of 1600-1620 ℃, wherein the temperature increase rate is 4-6 ℃/min, and when the target sintering temperature is reached, keeping the target sintering temperature for 3-4 h.
10. A silicon nitride-based ceramic body characterized in that the surface has a zirconium nitride coating; the composition mainly comprises the following components in percentage by weight: 60-85wt% of silicon nitride, 5-30wt% of zirconium dioxide and 5-20wt% of sintering aid.
CN202111262540.3A 2021-10-28 2021-10-28 Silicon nitride-based ceramic body and method for in-situ self-generating zirconium nitride coating on surface of silicon nitride-based ceramic Pending CN113880591A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101402449A (en) * 2008-06-30 2009-04-08 马北越 Process for producing zirconium nitride-silicon nitride composite powder
CN104098346A (en) * 2013-04-02 2014-10-15 中国科学院宁波材料技术与工程研究所 Preparation method of golden yellow zirconium nitride coating on base surface
CN105541341A (en) * 2016-01-12 2016-05-04 河北高富氮化硅材料有限公司 Method for preparing high-compactness silicon nitride ceramic by adding composite additives
WO2018061666A1 (en) * 2016-09-29 2018-04-05 三菱マテリアル電子化成株式会社 Zirconium nitride powder and method for producing same
CN111499392A (en) * 2020-04-24 2020-08-07 潍坊工商职业学院 High-hardness ceramic and preparation method thereof
CN112374897A (en) * 2020-03-20 2021-02-19 湖北中烟工业有限责任公司 Method for preparing silicon nitride ceramic by sintering under normal pressure

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101402449A (en) * 2008-06-30 2009-04-08 马北越 Process for producing zirconium nitride-silicon nitride composite powder
CN104098346A (en) * 2013-04-02 2014-10-15 中国科学院宁波材料技术与工程研究所 Preparation method of golden yellow zirconium nitride coating on base surface
CN105541341A (en) * 2016-01-12 2016-05-04 河北高富氮化硅材料有限公司 Method for preparing high-compactness silicon nitride ceramic by adding composite additives
WO2018061666A1 (en) * 2016-09-29 2018-04-05 三菱マテリアル電子化成株式会社 Zirconium nitride powder and method for producing same
CN112374897A (en) * 2020-03-20 2021-02-19 湖北中烟工业有限责任公司 Method for preparing silicon nitride ceramic by sintering under normal pressure
CN111499392A (en) * 2020-04-24 2020-08-07 潍坊工商职业学院 High-hardness ceramic and preparation method thereof

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Application publication date: 20220104