CN116023153B - Sintering method of silicon carbide ceramic - Google Patents
Sintering method of silicon carbide ceramic Download PDFInfo
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- CN116023153B CN116023153B CN202111238157.4A CN202111238157A CN116023153B CN 116023153 B CN116023153 B CN 116023153B CN 202111238157 A CN202111238157 A CN 202111238157A CN 116023153 B CN116023153 B CN 116023153B
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- 238000005245 sintering Methods 0.000 title claims abstract description 65
- 239000000919 ceramic Substances 0.000 title claims abstract description 43
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000001681 protective effect Effects 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 235000015895 biscuits Nutrition 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 239000002344 surface layer Substances 0.000 abstract description 5
- 238000005452 bending Methods 0.000 abstract description 3
- 238000005336 cracking Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000000280 densification Methods 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 238000001272 pressureless sintering Methods 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
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Abstract
The invention provides a sintering method of silicon carbide ceramics, which comprises the following steps: sintering in a positive pressure protective atmosphere, and then sintering in vacuum. The invention provides a sintering method of silicon carbide ceramic, which is particularly suitable for large-size block silicon carbide ceramic, solves the problems of sintering cracking, sintering clamping and non-densification in the prior art, and the overall density of the large-size block silicon carbide ceramic obtained by the sintering method is 3.05-3.18g/cm 3 The bending strength of the core part of the large-size block ceramic is 350-430MPa, and the core part has no obvious difference with the surface layer material.
Description
Technical Field
The invention belongs to the technical field of ceramic material forming, and particularly relates to a sintering method of silicon carbide ceramic, in particular to a sintering method of large-size block silicon carbide ceramic.
Background
The silicon carbide ceramic has the characteristics of high hardness, relatively low density, excellent elastic resistance, high cost performance and the like, so that the silicon carbide ceramic becomes an elastic-resistant ceramic material with the most development potential in the current generation. The pressureless sintered silicon carbide has high yield, can be prepared into complex shapes, and is the mainstream preparation method of the silicon carbide ceramics at present. The heat transfer in the pressureless sintering process is mainly carried out by radiation, and when a pressureless sintering process is adopted to fire a product with large thickness, the green body is heated from the surface layer to the inside, and the phenomenon of internal sintering or surface layer overburning often occurs. When the temperature rise rate is high, cracking is likely to occur. Therefore, the conventional pressureless sintering process is not an ideal method for firing large-sized bulk ceramics. So far, no application and related report of pressureless sintered silicon carbide ceramics with thickness of more than 40mm are seen.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a sintering method of silicon carbide ceramics, in particular to provide a sintering method of large-size block silicon carbide ceramics.
The invention provides a forming method of silicon carbide ceramic, which comprises the following steps: sintering in a positive pressure protective atmosphere, and then sintering in vacuum.
Preferably, the positive pressure protective atmosphere is Ar or N 2 。
Preferably, the pressure of the positive pressure protection is a micro positive pressure of between 100Pa and 9000Pa above 1 atmosphere.
Preferably, the vacuum degree of the vacuum sintering is 20Pa-100Pa.
Preferably, the positive pressure sintering temperature is 1800-2200 ℃, and the heat preservation time is 0-3h.
Preferably, the vacuum sintering temperature is 2100-2200 ℃, and the heat preservation time is 0.5-10h.
Preferably, the method comprises the following steps:
step 1, placing a silicon carbide ceramic biscuit into a carbon tube furnace, introducing protective gas, sintering at a positive pressure and a high temperature, and preserving heat;
step 2, cooling to 1400-1600 ℃, vacuum high-temperature sintering and heat preservation;
and 3, naturally cooling.
Preferably, the positive pressure protective atmosphere is Ar or N 2 The pressure of the positive pressure protection is micro positive pressure between 100Pa and 9000Pa above 1 atmosphere; the temperature of the positive pressure high-temperature sintering is 1800-2200 ℃, and the heat preservation time is 0-3h.
Preferably, the vacuum degree of the vacuum high-temperature sintering is 20Pa-100Pa; the temperature of the vacuum high-temperature sintering is 2100-2200 ℃, and the heat preservation time is 0.5-10h.
The beneficial effects are that:
the invention provides a sintering method of silicon carbide ceramic, which is particularly suitable for large-size block silicon carbide ceramic, solves the problems of sintering cracking, sintering clamping and non-densification in the prior art, and the overall density of the large-size block silicon carbide ceramic obtained by the sintering method is 3.05-3.18g/cm 3 The bending strength of the core part of the large-size block ceramic is 350-430MPa, and the core part has no obvious difference with the surface layer material.
Detailed Description
The invention is further illustrated by the following embodiments, which are to be understood as merely illustrative of the invention and not limiting thereof. Unless otherwise specified, each percentage refers to a mass percent.
The invention provides a sintering method of silicon carbide ceramics, which is particularly suitable for large-size block silicon carbide ceramics, and comprises the following steps:
step 1, placing a silicon carbide ceramic biscuit into a carbon tube furnace, introducing protective gas, sintering at a positive pressure and a high temperature, and preserving heat;
step 2, cooling to 1400-1600 ℃, vacuum high-temperature sintering and heat preservation;
and 3, naturally cooling.
In one embodiment, the positive pressure protective atmosphere is Ar or N 2 The pressure of the positive pressure protection is micro positive pressure between 100Pa and 9000Pa above 1 atmosphere; the temperature of the positive pressure high-temperature sintering is 1800-2200 ℃, and the heat preservation time is 0-3h.
In one embodiment, the vacuum degree of the vacuum high-temperature sintering is 20Pa-100Pa; the temperature of the vacuum high-temperature sintering is 2100-2200 ℃, and the heat preservation time is 0.5-10h.
The present invention will be further illustrated by the following examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, since numerous insubstantial modifications and variations will now occur to those skilled in the art in light of the foregoing disclosure. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Example 1:
placing the de-bonded large-size block silicon carbide ceramic biscuit into a carbon tube furnace, introducing Ar gas, sintering at high temperature to 1800 ℃ under the pressure of 800Pa higher than atmospheric pressure in the furnace, and preserving heat for 2h. Then cooling to 1500 ℃ and then carrying out vacuum sintering, wherein the vacuum degree in the furnace is 50Pa, heating to 2150 ℃, preserving heat for 2 hours, and then naturally cooling.
Example 2:
placing the de-bonded large-size block silicon carbide ceramic biscuit into a carbon tube furnace, and introducing N 2 The air pressure in the furnace is more than 800Pa, the sintering temperature is high to 2000 ℃, and the heat preservation is carried out for 2 hours. Then cooling to 1500 ℃ and then carrying out vacuum sintering, wherein the vacuum degree in the furnace is 50Pa, heating to 2150 ℃, preserving heat for 2 hours, and then naturally cooling.
Example 3:
placing the de-bonded large-size block silicon carbide ceramic biscuit into a carbon tube furnace, introducing Ar gas, sintering at high temperature to 2200 ℃ under the pressure of 800Pa higher than atmospheric pressure, and preserving the heat for 0h. Then cooling to 1500 ℃, performing vacuum sintering, heating to 2200 ℃ with the vacuum degree in the furnace of 50Pa, preserving heat for 10 hours, and naturally cooling.
Example 4:
placing the de-bonded large-size block silicon carbide ceramic biscuit into a carbon tube furnace, introducing Ar gas, sintering at high temperature to 2200 ℃ under the pressure of 9000Pa which is higher than atmospheric pressure, and preserving heat for 0h. Then cooling to 1500 ℃ and then carrying out vacuum sintering, wherein the vacuum degree in the furnace is 100Pa, heating to 2200 ℃, preserving heat for 5 hours, and then naturally cooling.
Example 5:
placing the de-bonded large-size block silicon carbide ceramic biscuit into a carbon tube furnace, introducing Ar gas, sintering at high temperature to 1900 ℃ under the pressure of 5000Pa higher than atmospheric pressure in the furnace, and preserving heat for 0h. Then cooling to 1500 ℃, performing vacuum sintering, heating to 2200 ℃ with the vacuum degree in the furnace of 20Pa, preserving heat for 5 hours, and naturally cooling.
Example 6:
placing the de-bonded large-size block silicon carbide ceramic biscuit into a carbon tube furnace, introducing Ar gas, sintering at a high temperature to 2100 ℃ under the pressure of 100Pa higher than the atmospheric pressure in the furnace, and preserving the heat for 3 hours. Then cooling to 1500 ℃, performing vacuum sintering, heating to 2100 ℃ with the vacuum degree in the furnace of 20Pa, preserving heat for 0.5h, and naturally cooling.
Example 7:
placing the de-bonded large-size block silicon carbide ceramic biscuit into a carbon tube furnace, and introducing N 2 And (3) sintering the gas at a high temperature to 2100 ℃ under the pressure of the furnace being greater than 1000Pa, and preserving the heat for 3 hours. Then cooling to 1500 ℃, performing vacuum sintering, wherein the vacuum degree in the furnace is 50Pa, heating to 2100 ℃, preserving heat for 6 hours, and then naturally cooling.
Example 8:
placing the de-bonded large-size block silicon carbide ceramic biscuit into a carbon tube furnace, introducing Ar gas, sintering at a high temperature to 2100 ℃ under the pressure of 5000Pa higher than the atmospheric pressure in the furnace, and preserving the heat for 1h. Then cooling to 1500 ℃ and then carrying out vacuum sintering, wherein the vacuum degree in the furnace is 60Pa, heating to 2150 ℃, preserving heat for 10 hours, and then naturally cooling.
Comparative examples:
placing the de-bonded large-size block silicon carbide ceramic biscuit into a carbon tube furnace, introducing Ar gas, sintering at high temperature to 2100 ℃, preserving heat for 10 hours, and then naturally cooling.
The sintered size and performance parameters of the silicon carbide green compacts obtained in the above examples are shown in Table 1.
TABLE 1
As can be seen from Table 1, the bulk density of the large-size bulk silicon carbide ceramic obtained by the sintering method of the invention is 3.05-3.18g/cm 3 The bending strength of the core part of the large-size block ceramic is 350-430MPa, and the core part has no obvious difference with the surface layer material. Comparative example the size of the silicon carbide ceramic green body was the same as that of example 1, and the density and flexural strength of the large-size bulk silicon carbide ceramic of example 1 using the sintering method of the present invention were improved, and the core and skin layer differences were greatly reduced.
Claims (4)
1. A method of sintering silicon carbide ceramic, comprising: sintering in a positive pressure protective atmosphere, and then sintering in vacuum;
the method specifically comprises the following steps:
step 1, placing a silicon carbide ceramic biscuit into a carbon tube furnace, introducing protective gas, sintering at a positive pressure and a high temperature, and preserving heat;
step 2, cooling to 1400-1600 ℃, and then sintering at a vacuum high temperature, and preserving heat;
step 3, naturally cooling;
the pressure of the positive pressure protection is micro positive pressure between 100Pa and 9000Pa above 1 atmosphere;
the temperature of the positive pressure high-temperature sintering is 1800-2200 ℃;
the vacuum degree of the vacuum high-temperature sintering is 20Pa-100Pa, and the temperature is 2100 ℃ to 2200 ℃.
2. The method for sintering silicon carbide ceramic according to claim 1, wherein the positive pressure protective atmosphere is Ar or N 2 。
3. The method for sintering silicon carbide ceramic according to claim 1, wherein the heat-retaining time of the positive pressure high-temperature sintering is 1 to 3 hours.
4. The method for sintering silicon carbide ceramic according to claim 1, wherein the vacuum high temperature sintering has a holding time of 0.5 to 10 hours.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5139719A (en) * | 1989-08-10 | 1992-08-18 | The British Petroleum Company P.L.C. | Sintering process and novel ceramic material |
| CN109665849A (en) * | 2019-01-09 | 2019-04-23 | 山东中鹏特种陶瓷有限公司 | Silicon carbide rotator and manufacturing process |
| CN111574226A (en) * | 2020-05-26 | 2020-08-25 | 潍坊盛润特种陶瓷有限公司 | Preparation method of high-density low-free silicon content reaction sintered silicon carbide ceramic material |
| CN111848174A (en) * | 2020-07-30 | 2020-10-30 | 山东中鹏特种陶瓷有限公司 | Method for producing wear-resistant silicon carbide ceramic block based on press machine |
| CN111908933A (en) * | 2020-07-30 | 2020-11-10 | 山东中鹏特种陶瓷有限公司 | Preparation method of large-size sintered silicon carbide wear-resistant pipeline |
-
2021
- 2021-10-25 CN CN202111238157.4A patent/CN116023153B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5139719A (en) * | 1989-08-10 | 1992-08-18 | The British Petroleum Company P.L.C. | Sintering process and novel ceramic material |
| CN109665849A (en) * | 2019-01-09 | 2019-04-23 | 山东中鹏特种陶瓷有限公司 | Silicon carbide rotator and manufacturing process |
| CN111574226A (en) * | 2020-05-26 | 2020-08-25 | 潍坊盛润特种陶瓷有限公司 | Preparation method of high-density low-free silicon content reaction sintered silicon carbide ceramic material |
| CN111848174A (en) * | 2020-07-30 | 2020-10-30 | 山东中鹏特种陶瓷有限公司 | Method for producing wear-resistant silicon carbide ceramic block based on press machine |
| CN111908933A (en) * | 2020-07-30 | 2020-11-10 | 山东中鹏特种陶瓷有限公司 | Preparation method of large-size sintered silicon carbide wear-resistant pipeline |
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