CN116425555A - Silicon nitride ceramic cutter and preparation method thereof - Google Patents
Silicon nitride ceramic cutter and preparation method thereof Download PDFInfo
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- CN116425555A CN116425555A CN202310117483.2A CN202310117483A CN116425555A CN 116425555 A CN116425555 A CN 116425555A CN 202310117483 A CN202310117483 A CN 202310117483A CN 116425555 A CN116425555 A CN 116425555A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 90
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 80
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 92
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003825 pressing Methods 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 238000007873 sieving Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000005507 spraying Methods 0.000 claims abstract description 4
- 238000009694 cold isostatic pressing Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 229910052582 BN Inorganic materials 0.000 claims description 7
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 238000007731 hot pressing Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 238000000465 moulding Methods 0.000 claims 2
- 238000005452 bending Methods 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
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- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
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- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
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- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
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Abstract
The invention belongs to the technical field of silicon nitride ceramics, and particularly relates to a silicon nitride ceramic cutter and a preparation method thereof, wherein the preparation method comprises the following steps: firstly, weighing the following components in percentage by weight: 75% -85% of silicon nitride powder, 10% -16% of pre-oxidized silicon nitride powder and ZrO 2 ‑Y 2 O 3 Mixing 5% -10% of the powder with water and ethanol to prepare ceramic slurry; spraying the ceramic slurry in hot air flow, granulating, drying, grinding and sieving to obtain ceramic powder;pressing and forming ceramic powder to obtain a ceramic blank; sintering the ceramic blank to obtain the silicon nitride ceramic cutter, wherein the Vickers hardness of the obtained silicon nitride ceramic cutter is 21.6-27.5GPa, and the fracture toughness is 12.7-15.8MPa m 1/2 The bending strength is 1053-1290MPa.
Description
Technical Field
The invention belongs to the technical field of silicon nitride ceramics, and particularly relates to a silicon nitride ceramic cutter and a preparation method thereof.
Background
Silicon nitride ceramics are one of ideal cutting tool materials for high-temperature alloy and bearing steel materials because of the high Vickers hardness, abrasion resistance, good high-temperature mechanical properties, oxidation resistance, thermal shock resistance and the like. Silicon nitride ceramics are generally prepared with high purity Si 3 N 4 The powder is used as raw material, and sintering aid is added to promote densification. However, in the research, the addition of the sintering aid can improve the mechanical properties of the silicon nitride ceramic, but the method is difficult to further improve the mechanical properties, and is difficult to meet the application of scenes with higher requirements.
In addition, at present, the silicon nitride ceramic cutter is usually prepared by grinding a ceramic material into the shape of the cutter, but the mode is easy to cause microcracking on the surface and the subsurface, so that the strength of the cutter is reduced, and the cutter is also formed by dry-pressing ceramic powder into the shape of the cutter in a cold isostatic pressing mode, but the pressure of dry-pressing is usually only tens of megapascals, the pressure is difficult to further improve, the density of a formed blank is lower, the mechanical property of the obtained cutter cannot meet the requirement, the pressure of the cold isostatic pressing can reach hundreds of megapascals, the density of the formed blank is higher, the cutter has high strength, but the shape of the ceramic blank formed by the cold isostatic pressing is usually regular, and the shape of the surface is difficult to be pressed into the blank with teeth or grooves, so that the application of the cold isostatic pressing is limited.
Disclosure of Invention
The invention provides a preparation method of a silicon nitride ceramic cutter, and the obtained ceramic material has higher density, high vickers hardness, fracture toughness and bending strength.
Based on the purposes, the silicon nitride ceramic cutter provided by the invention is mainly prepared from the following raw materials in percentage by weight:
75% -85% of silicon nitride powder, 10% -16% of pre-oxidized silicon nitride powder and ZrO 2 -Y 2 O 3 5% -10% of powder.
Optionally, the silicon nitride ceramic cutter comprises the following components in percentage by weight:
79.5% of silicon nitride powder, 13% of pre-oxidized silicon nitride powder and ZrO 2 4.72% of powder, Y 2 O 3 2.78% of powder.
Optionally, the oxygen content of the pre-oxidized silicon nitride powder is 3.8-5.2wt% and the thickness of the oxide layer is 0.02-0.06 mu m.
Optionally, the ceramic powder has a particle size of 1-8 μm.
Optionally, the ZrO 2 -Y 2 O 3 ZrO2 and Y in the powder 2 O 3 The mass ratio is (1.5-2) 1.
The preparation method of the silicon nitride ceramic cutter comprises the following steps:
firstly, weighing the following components in percentage by weight: silicon nitride powder, pre-oxidized silicon nitride powder, zrO 2 Powder and Y 2 O 3 Stirring the powder with water and ethanol to prepare ceramic slurry; spraying the ceramic slurry in hot air flow, granulating, drying, grinding and sieving to obtain ceramic powder; pressing and forming ceramic powder to obtain a ceramic blank; and sintering the ceramic blank to obtain the silicon nitride ceramic cutter.
Optionally, the preparation method of the pre-oxidized silicon nitride powder comprises the following steps:
and (3) reacting the silicon nitride powder in a high-pressure oxygen atmosphere at 750-900 ℃, cooling, and sieving to obtain the pre-oxidized silicon nitride powder.
Optionally, the method of press forming includes the steps of:
putting the ceramic powder into a die, and adopting a special-shaped surface pressure head to carry out dry pressing forming to obtain a dry pressed green body, wherein the upper surface structure of the dry pressed green body corresponds to the end face of the special-shaped surface pressure head, and the upper surface of the dry pressed green body is smooth; then covering boron nitride powder or graphite powder above the dry-pressed green body to level the upper end surface, and adopting a pressure head with a planar end part for secondary dry-pressing forming; and then adopting cold isostatic pressing to obtain a ceramic blank.
Optionally, in the ceramic body forming method, the pressure of the two dry pressing forming is 16-20MPa, and the pressure is maintained for 5-10min; the pressure of the cold isostatic pressing is 150-300MPa, and the pressure is maintained for 1-5min.
Optionally, the conditions for sintering the ceramic body are: hot-pressing sintering under inert gas atmosphere, wherein the sintering temperature is 1700-1900 ℃, the heat preservation time is 1-3 hours, and the sintering pressure is not more than 20MPa.
The beneficial effects of the invention are as follows: the Vickers hardness of the silicon nitride ceramic cutter obtained by the invention is 21.6-27.5GPa, and the fracture toughness is 12.7-15.8 MPa.m 1/2 The bending strength is 1053-1290MPa, and the mechanical property of the ceramic cutter is improved and then reduced along with the increase of the content of the pre-oxidized silicon nitride powder. ZrO (ZrO) 2 -Y 2 O 3 ZrO in powder 2 And Y is equal to 2 O 3 The mass ratio is controlled to be (1.5-2) 1, zrO 2 And Y is equal to 2 O 3 When the mass ratio is 1.7:1, the obtained silicon nitride ceramic cutter obviously improves the fracture toughness and further improves the comprehensive performance under the condition that the reduction of the Vickers hardness and the bending strength is not obvious.
According to the preparation method of the silicon nitride ceramic cutter, the special-shaped surface pressure head is adopted for dry pressing forming, so that a dry pressed green body is obtained, the upper surface structure of the dry pressed green body corresponds to the end face of the special-shaped surface pressure head, and the upper surface of the dry pressed green body is smooth; the upper part of the dry pressed green body is covered with boron nitride powder or graphite powder, the boron nitride powder or the graphite powder fills the toothed groove or the groove of the green body, and a pressure head with a plane end is adopted for secondary dry pressing forming, so that the upper surface of the dry pressed green body is flat and regular, other surfaces are in contact with a die and are flat and regular, the ceramic green body can be obtained by adopting cold isostatic pressing, the ceramic green body with the toothed groove or the groove has higher compactness, and the special-shaped cutter with good mechanical property is beneficial to obtaining.
Detailed Description
The present invention will be further described in detail below with reference to specific embodiments and with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent.
Example 1
The preparation method of the silicon nitride ceramic cutter comprises the following steps:
s1, weighing the following components in percentage by weight: 79.5% of silicon nitride powder, 10% of pre-oxidized silicon nitride powder and ZrO 2 5% of powder Y 2 O 3 Mechanically stirring 2.5% of powder with water and ethanol to prepare ceramic slurry;
s2, spraying the ceramic slurry in hot air at 100 ℃, granulating, drying at 100 ℃ for 10 hours, grinding and sieving to obtain ceramic powder;
s3, placing the ceramic powder into a die, and performing dry pressing forming by adopting a special-shaped surface pressure head to obtain a dry pressed green body, wherein the upper surface structure of the dry pressed green body corresponds to the end face of the special-shaped surface pressure head, and the upper surface of the dry pressed green body is smooth; then covering boron nitride powder above the dry-pressed green body, adopting a pressure head with a plane end for secondary dry-pressing forming to enable the upper end surface to be flat, keeping the pressure of the secondary dry-pressing forming at 16MPa for 6min; then adopting cold isostatic pressing to obtain a ceramic blank, wherein the pressure of the cold isostatic pressing is 150-300MPa, and the pressure is maintained for 2min;
and S4, hot-pressing and sintering the ceramic blank in a nitrogen gas atmosphere, wherein the sintering temperature is 1800 ℃, the heat preservation time is 2 hours, and the sintering pressure is 15MPa, so that the silicon nitride ceramic cutter is obtained.
Example 2
S1, weighing the following components in percentage by weight: 79.5% of silicon nitride powder, 13% of pre-oxidized silicon nitride powder and ZrO 2 5% of powder Y 2 O 3 Mechanically stirring 2.5% of powder with water and ethanol to prepare ceramic slurry; the remaining steps were the same as in example 1.
Example 3
S1, weighing the following components in percentage by weight: 79.5% of silicon nitride powder, 16% of pre-oxidized silicon nitride powder and ZrO 2 5% of powder Y 2 O 3 Mechanically stirring 2.5% of powder with water and ethanol to prepare ceramic slurry; the remaining steps were the same as in example 1.
Example 4
S1, weighing the following components in percentage by weight: 79.5% of silicon nitride powder, 13% of pre-oxidized silicon nitride powder and ZrO 2 4.5% of powder, Y 2 O 3 3% of the powder is mechanically stirred with water and ethanol,preparing ceramic slurry; the remaining steps were the same as in example 1.
Example 5
S1, weighing the following components in percentage by weight: 79.5% of silicon nitride powder, 13% of pre-oxidized silicon nitride powder and ZrO 2 4.72% of powder, Y 2 O 3 Mechanically stirring 2.78% of powder with water and ethanol to prepare ceramic slurry; the remaining steps were the same as in example 1.
Comparative example 1
S1, weighing the following components in percentage by weight: 92.5% of silicon nitride powder and ZrO 2 4.5% of powder, Y 2 O 3 Mechanically stirring 3% of powder with water and ethanol to prepare ceramic slurry; the remaining steps were the same as in example 1.
Comparative example 2
S1, weighing the following components in percentage by weight: 79.5% of silicon nitride powder, 13% of pre-oxidized silicon nitride powder and ZrO 2 Mechanically stirring 7.5% of powder with water and ethanol to prepare ceramic slurry; the remaining steps were the same as in example 1.
Comparative example 3
S1, weighing the following components in percentage by weight: 79.5% of silicon nitride powder, 13% of pre-oxidized silicon nitride powder and Y 2 O 3 Mechanically stirring 7.5% of powder with water and ethanol to prepare ceramic slurry; the remaining steps were the same as in example 1.
The samples of the silicon nitride ceramic tools prepared in the above groups were subjected to mechanical property tests, and the test data of each sample are shown in table 1 below:
TABLE 1
As is clear from Table 1, the silicon nitride ceramic tools prepared in examples 1 to 5 of the present invention have a Vickers hardness of 21.6 to 27.5GPa and a fracture toughness of 12.7 to 15.8MPa m 1/2 Flexural strength of 1053-1290MPa, according to examples 1-3, the mechanical properties of the ceramic tool are improved and then reduced as the content of the pre-oxidized silicon nitride powder is increased. As can be seen from examples 2, 4 and 5, zrO 2 -Y 2 O 3 ZrO in powder 2 And Y is equal to 2 O 3 The mass ratio is controlled to be (1.5-2) 1, zrO 2 And Y is equal to 2 O 3 When the mass ratio is 1.7:1, the obtained silicon nitride ceramic cutter obviously improves the fracture toughness and further improves the comprehensive performance under the condition that the reduction of the Vickers hardness and the bending strength is not obvious.
In comparative example 1, the mechanical properties of the silicon nitride ceramic tool without the pre-oxidized silicon nitride powder are obviously lower than those of each example; in comparative example 2, Y was not added 2 O 3 The mechanical properties of the powder and the silicon nitride ceramic cutter are obviously lower than those of the embodiments; in comparative example 2, no ZrO was added 2 The mechanical properties of the powder and the silicon nitride ceramic cutter are obviously lower than those of the embodiments; and the mechanical properties of the ceramic cutters obtained in comparative examples 1-3 are obviously reduced.
According to the preparation method of the silicon nitride ceramic cutter, the special-shaped surface pressure head is adopted for dry pressing forming, so that a dry pressed green body is obtained, the upper surface structure of the dry pressed green body corresponds to the end face of the special-shaped surface pressure head, and the upper surface of the dry pressed green body is smooth; the upper part of the dry pressed green body is covered with boron nitride powder or graphite powder, the boron nitride powder or the graphite powder fills the toothed groove or the groove of the green body, and a pressure head with a plane end is adopted for secondary dry pressing forming, so that the upper surface of the dry pressed green body is flat and regular, other surfaces are in contact with a die and are flat and regular, the ceramic green body can be obtained by adopting cold isostatic pressing, the ceramic green body with the toothed groove or the groove has higher compactness, and the special-shaped cutter with good mechanical property is beneficial to obtaining.
Those of ordinary skill in the art will appreciate that: the discussion of any of the embodiments above is merely exemplary and is not intended to imply that the scope of the present application is limited to such examples; the technical features of the above embodiments or in the different embodiments may also be combined under the idea of the present application, the steps may be implemented in any order, and there are many other variations of the different aspects of one or more embodiments in the present application as described above, which are not provided in details for the sake of brevity.
One or more embodiments herein are intended to embrace all such alternatives, modifications and variations that fall within the broad scope of the present application. Any omissions, modifications, equivalents, improvements, and the like, which are within the spirit and principles of the one or more embodiments in the present application, are therefore intended to be included within the scope of the present application.
Claims (10)
1. The silicon nitride ceramic cutter is characterized by being mainly prepared from the following raw materials in percentage by weight:
75% -85% of silicon nitride powder, 10% -16% of pre-oxidized silicon nitride powder and ZrO 2 -Y 2 O 3 5% -10% of powder.
2. The silicon nitride ceramic tool according to claim 1, comprising the following components in weight percent:
79.5% of silicon nitride powder, 13% of pre-oxidized silicon nitride powder and ZrO 2 4.72% of powder, Y 2 O 3 2.78% of powder.
3. A silicon nitride ceramic tool according to claim 1, wherein the pre-oxidized silicon nitride powder has an oxygen content of 3.8-5.2wt% and an oxide layer thickness of 0.02-0.06 μm.
4. The silicon nitride ceramic tool according to claim 1, wherein the ceramic powder has a particle size of 1-8 μm.
5. The silicon nitride ceramic tool according to claim 1, wherein the ZrO 2 -Y 2 O 3 ZrO2 and Y in the powder 2 O 3 The mass ratio is (1.5-2) 1.
6. A method of producing a silicon nitride ceramic tool according to any one of claims 1 to 5, comprising the steps of:
firstly, weighing the following components in percentage by weight: silicon nitride powder, pre-oxidized silicon nitride powder, zrO 2 Powder and Y 2 O 3 Stirring the powder with water and ethanol to prepare ceramic slurry; spraying the ceramic slurry in hot air flow, granulating, drying, grinding and sieving to obtain ceramic powder; pressing and forming ceramic powder to obtain a ceramic blank; and sintering the ceramic blank to obtain the silicon nitride ceramic cutter.
7. The method of producing a silicon nitride ceramic tool according to claim 6, wherein the method of producing a pre-oxidized silicon nitride powder comprises the steps of:
and (3) reacting the silicon nitride powder in a high-pressure oxygen atmosphere at 750-900 ℃, cooling, and sieving to obtain the pre-oxidized silicon nitride powder.
8. The method of manufacturing a silicon nitride ceramic tool according to claim 6, wherein the method of press forming comprises the steps of:
putting the ceramic powder into a die, and adopting a special-shaped surface pressure head to carry out dry pressing forming to obtain a dry pressed green body, wherein the upper surface structure of the dry pressed green body corresponds to the end face of the special-shaped surface pressure head, and the upper surface of the dry pressed green body is smooth; then covering boron nitride powder or graphite powder above the dry-pressed green body to level the upper end surface, and adopting a pressure head with a planar end part for secondary dry-pressing forming; and then adopting cold isostatic pressing to obtain a ceramic blank.
9. The method for manufacturing a silicon nitride ceramic tool according to claim 6, wherein in the ceramic body molding method, the pressure of the two dry press molding is 16-20MPa, and the pressure is maintained for 5-10min; the pressure of the cold isostatic pressing is 150-300MPa, and the pressure is maintained for 1-5min.
10. The method for manufacturing a silicon nitride ceramic tool according to claim 6, wherein the conditions for sintering the ceramic body are: hot-pressing sintering under inert gas atmosphere, wherein the sintering temperature is 1700-1900 ℃, the heat preservation time is 1-3 hours, and the sintering pressure is not more than 20MPa.
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