CN117886612A - High-wear-resistance silicon nitride ceramic and preparation method and application thereof - Google Patents
High-wear-resistance silicon nitride ceramic and preparation method and application thereof Download PDFInfo
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- CN117886612A CN117886612A CN202311820343.8A CN202311820343A CN117886612A CN 117886612 A CN117886612 A CN 117886612A CN 202311820343 A CN202311820343 A CN 202311820343A CN 117886612 A CN117886612 A CN 117886612A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 72
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 64
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 23
- 239000011812 mixed powder Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 238000005299 abrasion Methods 0.000 claims description 21
- 239000002904 solvent Substances 0.000 claims description 18
- 239000006229 carbon black Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 239000003054 catalyst Substances 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 5
- 238000000227 grinding Methods 0.000 description 9
- 238000011068 loading method Methods 0.000 description 5
- 239000011805 ball Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of preparation of silicon nitride ceramics, and discloses a high-wear-resistance silicon nitride ceramic, and a preparation method and application thereof. The method comprises the step of adding high-entropy carbonitride (Ti 0.2 Ta 0.2 Nb 0.2 Mo 0.2 W 0.2 )(C n N 1‑n )，0.25≤n≤0.75、α‑Si 3 N 4 MgO and Re 2 O 3 Mixing, ball milling and drying to obtain mixed powder, sintering the mixed powder by discharge plasma, heating to 1600-1700 ℃ and preserving heat for 10-15 min to obtain the high wear-resistant silicon nitride ceramic. The invention leads alpha to‑Si 3 N 4 The powder is introduced with high-entropy carbonitride powder, and the prepared silicon nitride ceramic has excellent interface bonding and high wear resistance, and can be applied to ceramic bearing balls or cutting superhard cutters.
Description
Technical Field
The invention belongs to the technical field of preparation of silicon nitride ceramics, and discloses a high-wear-resistance silicon nitride ceramic, and a preparation method and application thereof.
Background
The silicon nitride ceramic has excellent performances such as low density, high hardness, high temperature resistance, high strength, low thermal expansion coefficient and the like, is structural ceramic with very good comprehensive performance, and is widely applied to the fields such as high-speed bearings, aerospace, refractory materials and the like. The ceramic prepared by taking the high-entropy carbonitride as a matrix has more excellent physical and chemical properties, including higher hardness, higher oxidation resistance and better wear resistance, is also high-performance structural ceramic, and has good application prospect in the structural ceramic fields of paint, high-temperature structural parts, cutters and the like. The high-entropy carbonitride powder is introduced into the raw material powder of the silicon nitride ceramic, so that the hardness of the silicon nitride ceramic can be improved, and the silicon nitride ceramic has higher wear resistance, so that the silicon nitride ceramic is widely applied to ceramic bearing balls and cutters for cutting superhard materials. Therefore, in order to realize the wide application of the high wear-resistant silicon nitride ceramic material, development of a method for preparing the high wear-resistant silicon nitride ceramic at low cost is urgently needed, so that the high wear-resistant silicon nitride ceramic material has high hardness and wear resistance.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the primary purpose of the invention is to provide a preparation method of high-wear-resistance silicon nitride ceramics. The method comprises the steps of self-synthesizing high-entropy carbonitride powder, and introducing the high-entropy carbonitride powder into alpha-Si 3 N 4 Adding sintering aids MgO and Re into the powder 2 O 3 And finally, carrying out spark plasma sintering to obtain the high-wear-resistance silicon nitride ceramic.
It is still another object of the present invention to provide a silicon nitride ceramic with high abrasion resistance produced by the above method.
It is a further object of the present invention to provide the use of the above-mentioned high wear resistant silicon nitride ceramics.
The aim of the invention is achieved by the following technical scheme:
a preparation method of high-wear-resistance silicon nitride ceramics comprises the following specific steps:
s1, tiO is prepared 2 MoO 3 WO 3 Ta 2 O 5 And Nb (Nb) 2 O 5 Mixing with carbon black, adding solvent and Si 3 N 4 Ball milling with ball milling medium, drying to obtain mixed powder A, molding the mixed powder A into blank, heating to 1600-1800 deg.c in nitrogen atmosphere of 1atm in pressureless furnace, heat treating and maintaining to obtain high entropy carbonitride (Ti) 0.2 Ta 0.2 Nb 0.2 Mo 0.2 W 0.2 )(C n N 1-n )0.25n0.75
S2, the high-entropy carbonitride and alpha-Si are processed 3 N 4 MgO and Re 2 O 3 Mixing, adding solvent and ball milling medium Si 3 N 4 Performing roller ball milling, drying and sieving to obtain mixed powder B,
s3, under the nitrogen atmosphere, the axial pressure is 10-50 MPa, the air pressure in the furnace is 20-30 mbar, the temperature of the mixed powder B is increased to 1600-1700 , and the mixed powder B is sintered by discharge plasma and is insulated, so that the high-wear-resistance silicon nitride ceramic is prepared.
Preferably, the TiO in step S1 2 MoO 3 WO 3 Ta 2 O 5 And Nb (Nb) 2 O 5 The particle size of the carbon black is 1-2 mu m, the particle size of the carbon black is 100-300 nm, and the purity is more than 99%.
Preferably, the solvent in step S1 is absolute ethanol or acetone; the mass ratio of the ball milling medium to the solvent to the mixed powder A is (7-10) 1:1, and the roller milling time is 12-24 hours;
the TiO 2 MoO 3 WO 3 Ta 2 O 5 Nb 2 O 5 And the mass ratio of the carbon black is (7.91-8.15): (14.24-14.68): (22.94-23.64): (21.86-22.53): (13.14-13.55): (19.91-17.45).
Preferably, the temperature rising rate in the step S1 is 5-20 /min, the heat preservation time is 1-2 h, and the average grain size of the high-entropy carbonitride is 400-600 nm.
Preferably, the -Si in step S2 3 N 4 Has a particle diameter of 300-500 nm and Re 2 O 3 Wherein Re is Dy, yb, ce, ho, pr or Lu, mgO particle size is 50-150 nm, re 2 O 3 The grain diameter is 3-6 mu m, and the purity is over 99 percent.
Preferably, the high entropy carbonitride, -Si, described in step S2 3 N 4 MgO and Re 2 O 3 The volume ratio of (5-7): (84-90): (3-5): (2-4) is Si 3 N 4 The ball is ball milling medium, and the solvent is absolute ethanol or acetone; si (Si) 3 N 4 The mass ratio of the ball milling medium, the solvent and the powder is (2-4) 1:1, and the roller ball milling time is 12-24 h.
Preferably, the temperature rising rate in the step S3 is 80-150 /min, and the heat preservation time is 10-15 min.
A high wear-resistant silicon nitride ceramic is prepared by the method.
Preferably, the silicon nitride ceramic has a friction coefficient of 0.3 to 0.4 and a wear rate of (2.3 to 3.1). Times.10 -6 mm 3 /Nm
The silicon nitride ceramic with high wear resistance is applied to ceramic bearing balls or cutting superhard cutters.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention is characterized in that alpha-Si 3 N 4 Adding high-entropy carbonitride (Ti) 0.2 Ta 0.2 Nb 0.2 Mo 0.2 W 0.2 )(C n N 1-n ) N is more than or equal to 0.25 and less than or equal to 0.75 to prepare high wear-resistant silicon nitride ceramics, and the ceramics simultaneously have higher toughness (fracture toughness is 8-9 MPa m) 1/2 ) And the higher hardness (the Vickers hardness is 22-25 GPa) of the high-entropy carbonitride ceramic.
2. The silicon nitride ceramics with high wear resistance prepared by the invention has extremely high frictional wear performance (the friction coefficient is 0.3-0.4, and the wear rate is 2.3 multiplied by 10) -6 3.110 -6 mm 3 /Nm)
Detailed Description
The present invention is further illustrated below in conjunction with specific examples, but should not be construed as limiting the invention. The technical means used in the examples are conventional means well known to those skilled in the art unless otherwise indicated. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Example 1
1. TiO with the mass ratio of 8.02:14.46:23.28:22.19:13.35:18.70 2 MoO 3 WO 3 Ta 2 O 5 Nb 2 O 5 Mixing with carbon black, with Si 3 N 4 Ball is ball milling medium, solvent is absolute ethyl alcohol, the mass ratio of grinding ball, solvent and mixed powder is 10:1:1, the mixed powder, grinding ball medium and solvent are placed in a ball milling tank, mixed ball milling is carried out on a roller ball mill for 24 hours, and after drying, the mixed powder A is obtained through a 200-mesh sieve.
2. The green body after the mixed powder A is molded is put into a graphite crucible and is placed into a pressureless furnace, and is heated to 1600 at a speed of 10 /min in a nitrogen atmosphere of 1atm, and is preserved for 2 hours, thus obtaining the high-entropy carbonitride (Ti) 0.2 Ta 0.2 Nb 0.2 Mo 0.2 W 0.2 )(C 0.5 N 0.5 ) The average particle diameter thereof was 400nm.
3. The volume fraction ratio (Ti 0.2 Ta 0.2 Nb 0.2 Mo 0.2 W 0.2 )(C 0.5 N 0.5 )-Si 3 N 4 MgO and Re 2 O 3 Mixing with Si 3 N 4 Ball milling medium, absolute ethyl alcohol as solvent, grinding ball, solvent and mixed powder in the mass ratio of 3 to 1, mixing the powder, grinding ball medium and solvent in ball milling tank, ball milling in roller ball mill for 24 hr, drying and sieving with 100 mesh sieve to obtain mixed powder B.
4. And (3) placing the mixed powder B into a discharge plasma sintering furnace for sintering, wherein the air pressure in the furnace is 30mbar, heating to 1650 at a speed of 100 /min under the nitrogen atmosphere, sintering, and preserving heat for 10min, wherein the axial compression in the heat preservation process is 30MPa, so that the high-wear-resistance silicon nitride ceramic is prepared.
For the high abrasion resistant silicon nitride ceramics prepared in the embodiment, the silicon nitride ceramics are adopted as grinding balls, and a ball-disc type frictional wear tester is adopted to carry out frictional wear test on the high abrasion resistant silicon nitride ceramics in dry air, the loading load is 1500g, the wear radius is 6mm, the rotating speed is 800r/min, the test time is 60min, and the measured friction coefficient of the high abrasion resistant silicon nitride ceramics is 0.3 and the wear rate is 2.3X10 -6 mm 3 /Nm
Example 2
The difference from example 1 is that: in step 3 (Ti) 0.2 Ta 0.2 Nb 0.2 Mo 0.2 W 0.2 )(C 0.5 N 0.5 )-Si 3 N 4 MgO and Re 2 O 3 The volume fraction ratio of (2) is 6:89:3:2, and the heat preservation temperature in the step 4 is 1700 , so that the high-wear-resistance silicon nitride ceramic is prepared.
For the high abrasion resistant silicon nitride ceramics prepared in the embodiment, the silicon nitride ceramics are adopted as grinding balls, and a ball-disc type frictional wear tester is adopted to carry out frictional wear test on the high abrasion resistant silicon nitride ceramics in dry air, the loading load is 1500g, the wear radius is 6mm, the rotating speed is 800r/min, the test time is 60min, and the measured friction coefficient of the high abrasion resistant silicon nitride ceramics is 0.3 and the wear rate is 3.1X10 -6 mm 3 /Nm
Example 3
The difference from example 1 is that: tiO in step 1 2 MoO 3 WO 3 Ta 2 O 5 Nb 2 O 5 And carbon black in a mass ratio of 7.91:14.24:22.94:21.86:13.14:19.91 to produce a high entropy carbonitride of (Ti 0.2 Ta 0.2 Nb 0.2 Mo 0.2 W 0.2 )(C 0.75 N 0.25 ) And 2, preserving heat for 1h at 1700 in the step 2 to obtain the high-wear-resistance silicon nitride ceramic.
For the silicon nitride ceramics with high wear resistance prepared in the embodiment, the silicon nitride ceramics are used as grinding balls, and the ball-disc type friction and wear tester is adopted to carry out friction and wear on the silicon nitride ceramics with high wear resistance in dry airThe test shows that the loading load is 1500g, the abrasion radius is 6mm, the rotating speed is 800r/min, the test time is 60min, the friction coefficient of the high abrasion-resistant silicon nitride ceramic is 0.35, and the abrasion rate is 2.8X10 -6 mm 3 /Nm
Example 4
The difference from example 1 is that: (Ti of step 3 0.2 Ta 0.2 Nb 0.2 Mo 0.2 W 0.2 )(C 0.5 N 0.5 )-Si 3 N 4 MgO and Re 2 O 3 The volume fraction ratio of (2) is 7:88:3:3, and the temperature in the step 4 is 1600 , so that the high-wear-resistance silicon nitride ceramic is prepared.
For the high abrasion resistant silicon nitride ceramics prepared in the embodiment, the silicon nitride ceramics are adopted as grinding balls, and a ball-disc type frictional wear tester is adopted to carry out frictional wear test on the high abrasion resistant silicon nitride ceramics in dry air, the loading load is 1500g, the wear radius is 6mm, the rotating speed is 800r/min, the test time is 60min, and the measured friction coefficient of the high abrasion resistant silicon nitride ceramics is 0.4 and the wear rate is 3.0x10 -6 mm 3 /Nm
Example 5
The difference from example 1 is that: and (3) the heating rate in the step (4) is 150 /min, the axial pressurization in the heat preservation process is 50MPa, and the high-wear-resistance silicon nitride ceramic is prepared.
For the high abrasion resistant silicon nitride ceramics prepared in the embodiment, the silicon nitride ceramics are adopted as grinding balls, and a ball-disc type frictional wear tester is adopted to carry out frictional wear test on the high abrasion resistant silicon nitride ceramics in dry air, the loading load is 1500g, the wear radius is 6mm, the rotating speed is 800r/min, the test time is 60min, and the measured friction coefficient of the high abrasion resistant silicon nitride ceramics is 0.3 and the wear rate is 2.4x10 -6 mm 3 /Nm
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the high-wear-resistance silicon nitride ceramic is characterized by comprising the following specific steps of:
s1, tiO is prepared 2 MoO 3 WO 3 Ta 2 O 5 And Nb (Nb) 2 O 5 Mixing with carbon black, adding solvent and Si 3 N 4 Ball milling with ball milling medium, drying to obtain mixed powder A, molding the mixed powder A into blank, heating to 1600-1800 deg.c in nitrogen atmosphere of 1atm in pressureless furnace, heat treating and maintaining to obtain high entropy carbonitride (Ti) 0.2 Ta 0.2 Nb 0.2 Mo 0.2 W 0.2 )(C n N 1-n )0.25n0.75
S2, the high-entropy carbonitride and alpha-Si are processed 3 N 4 MgO and Re 2 O 3 Mixing, adding solvent and ball milling medium Si 3 N 4 Performing roller ball milling, drying and sieving to obtain mixed powder B,
s3, under the nitrogen atmosphere, the axial pressure is 10-50 MPa, the air pressure in the furnace is 20-30 mbar, the temperature of the mixed powder B is increased to 1600-1700 , and the mixed powder B is sintered by discharge plasma and is insulated, so that the high-wear-resistance silicon nitride ceramic is prepared.
2. The method for producing a highly abrasion-resistant silicon nitride ceramic according to claim 1, wherein the TiO in step S1 is as follows 2 MoO 3 WO 3 Ta 2 O 5 And Nb (Nb) 2 O 5 The particle size of the carbon black is 1-2 mu m, the particle size of the carbon black is 100-300 nm, and the purity is more than 99%.
3. The method for producing a silicon nitride ceramic with high wear resistance according to claim 1, wherein the TiO in step S1 is 2 MoO 3 WO 3 Ta 2 O 5 Nb 2 O 5 The mass ratio of the carbon black to the catalyst is (7.91-8.15): (14.24-14.68): (22.94-23.64): (21.86-22.53)13.14 to 13.55 percent (19.91 to 17.45 percent), wherein the solvent is absolute ethyl alcohol or acetone; the mass ratio of the ball milling medium to the solvent to the mixed powder A is (7-10) 1:1, and the roller milling time is 12-24 h.
4. The method for producing a highly abrasion-resistant silicon nitride ceramic according to claim 1, wherein the rate of temperature rise in step S1 is 5 to 20 /min, the time for heat preservation is 1 to 2 hours, and the average grain size of the high-entropy carbonitride is 400 to 600nm.
5. The method for producing a highly abrasion-resistant silicon nitride ceramic according to claim 1, wherein the -Si in step S2 3 N 4 Has a particle diameter of 300-500 nm and Re 2 O 3 Wherein Re is Dy, yb, ce, ho, pr or Lu, mgO particle size is 50-150 nm, re 2 O 3 The grain diameter is 3-6 mu m, and the purity is over 99 percent.
6. The method for producing a highly abrasion-resistant silicon nitride ceramic according to claim 1, wherein the high entropy carbonitride, -Si, described in step S2 3 N 4 MgO and Re 2 O 3 The volume ratio of (5-7): (84-90): (3-5): (2-4) is Si 3 N 4 The ball is ball milling medium, and the solvent is absolute ethanol or acetone; si (Si) 3 N 4 The mass ratio of the ball milling medium, the solvent and the powder is (2-4) 1:1, and the roller ball milling time is 12-24 h.
7. The method for preparing high wear-resistant silicon nitride ceramic according to claim 1, wherein the heating rate in step S3 is 80-150 /min, and the time for heat preservation is 10-15 min.
8. A highly wear resistant silicon nitride ceramic prepared by the method of any one of claims 1-7.
9. According toThe highly abrasion-resistant silicon nitride ceramic according to claim 1, wherein the silicon nitride ceramic has a coefficient of friction of 0.3 to 0.4 and a wear rate of (2.3 to 3.1). Times.10 -6 mm 3 /Nm
10. Use of a highly wear resistant silicon nitride ceramic as claimed in claim 8 or 9 in a ceramic bearing ball or a cutting superhard cutter.
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