CN103073334A - Preparation method for ultralong nanowire toughed ceramic coating - Google Patents
Preparation method for ultralong nanowire toughed ceramic coating Download PDFInfo
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- CN103073334A CN103073334A CN2013100214612A CN201310021461A CN103073334A CN 103073334 A CN103073334 A CN 103073334A CN 2013100214612 A CN2013100214612 A CN 2013100214612A CN 201310021461 A CN201310021461 A CN 201310021461A CN 103073334 A CN103073334 A CN 103073334A
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Abstract
The invention relates to a preparation method for an ultralong nanowire toughed ceramic coating. An anti-oxidation ceramic coating made from a C/C composite material is toughened by adopting an ultralong SiC nanowire, and a load in a base body can be effectively transferred onto the nanowire by higher length-diameter ratio of the nanowire, so that the toughness of the ceramic coating is enhanced, the cracking trend of the ceramic coating is weakened, and the oxidation resistance of the ceramic coating is improved at last. Compared with the prior art, the prepared SiC nanowire toughened ceramic coating can be used for effectively preventing the C/C composite material from being oxidized. The research result shows that a coating test piece is kept in a weight gain state all the time in a thermogravimetry test process at a room temperature of 1500 DEG C, and the maximum weight gain rate is 1.21%-1.43%.
Description
Technical field
The present invention relates to a kind of preparation method of overlong nanowire toughening ceramic coating, be specifically related to the preparation method of the toughness reinforcing carbon/carbon of a kind of ultralong SiC nanowires (C/C) composite material antioxidation ceramic coating.
Background technology
The easy oxidation of high temperature is the C/C matrix material as the thermal structure material bottleneck problem of difficult breakthrough in actual applications.The investigator has proposed many solutions both at home and abroad, and wherein, the ceramic coating technology is the effective means that solves C/C matrix material high temperature easy-oxidizing hard topic.Yet, in the application process of reality, easily do not cause coating in high low temperature alternation process, to ftracture because the thermal expansivity between ceramic coating and the C/C matrix does not mate, and then reduce its anti-aging capability.In order to have alleviated the cracking trend of ceramic coating, nanowire-toughened ceramic coating technology has caused researchist's very big concern.
Document " Oxidation protection of C/C composites with a multilayer coating of SiC and Si+SiC+SiC nanowires; Chu Yanhui; Li Hejun; Fu Qiangang; Wang Haipeng; Hou Xianghui, Zou Xu, Shang Gunan.Carbon2012 (50): 1280-1288 " has been introduced the cracking trend that a kind of technology that adopts the nanowire-toughened C/C composite material ceramic coating of traditional Si C is alleviated ceramic coating.Although this technology has been alleviated the cracking trend of ceramic coating in high low temperature alternation process to a certain extent, improved the anti-aging capability of ceramic coating to the C/C matrix material, but the lower length-to-diameter ratio of traditional nano wire self has limited its toughening effect in ceramic coating.Therefore, the coating of preparation still ftractures in the process of high low temperature alternation easily, and finally causing it is not very desirable to C/C composite material antioxidation ability.Result of study shows: coating specimens is in the thermogravimetric process of the test of room temperature to 1500 ° C, and maximum rate of weight loss reaches 0.86%.
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes a kind of preparation method of overlong nanowire toughening ceramic coating, can reduce the cracking trend of ceramic coating in high low temperature alternation process, improves the anti-aging capability of ceramic coating.
Technical scheme
A kind of preparation method of overlong nanowire toughening ceramic coating is characterized in that step is as follows:
Step 1: with cleaning behind the C/C matrix material sanding and polishing, then put into baking oven and dry;
Step 2: take by weighing mass percent and be 60～85% Si powder, 5～15% SiC powder, 7～15% C powder and 3～10% Al
2O
3Powder places ball grinder, the powder that ball milling combination treatment 2～4h obtains mixing;
Step 3: the part powder is laid in the plumbago crucible, puts into again the C/C matrix material of oven dry, cover again on the C/C matrix material and establish the part powder;
Step 4: plumbago crucible is put into the pyroreaction sintering oven, with 5～10 ° of C/min heat-up rates furnace temperature is risen to 2000～2200 ° of C from room temperature, insulation 1～3h; Powered-down naturally cools to room temperature subsequently, and omnidistance Ar gas protection obtains the C/C matrix material with ceramic coating;
Step 5: Graphite Powder 99 is put into plumbago crucible, make its even bedding in crucible bottom, will bundle with the C/C matrix material of ceramic coating above the Graphite Powder 99 of rear-mounted in crucible again;
Step 6: plumbago crucible is put into the pyroreaction sintering oven, with 5～10 ° of C/min heat-up rates furnace temperature is risen to 1400～1600 ° of C from room temperature, insulation 1～3h; Powered-down naturally cools to room temperature subsequently, and logical Ar protection in the whole process obtains the surface with the C/C matrix material of the ceramic coating coating of ultralong SiC nanowires;
Step 7: the part powder of step 2 preparation is laid in the plumbago crucible, puts into again the C/C matrix material that the surface coats with the ceramic coating of ultralong SiC nanowires, again the cover part powder;
Step 8: plumbago crucible is put into the pyroreaction sintering oven, with 5～10 ° of C/min heat-up rates furnace temperature is risen to 2000～2200 ° of C from room temperature, insulation 1～3h; Powered-down naturally cools to room temperature subsequently, and logical argon shield obtains overlong nanowire toughening ceramic coating at the C/C composite material surface in the whole process.
Part powder in described step 3 and the step 7 is 1/4 of powder.
Adopt a branch of 3k carbon fiber binding C/C matrix material to be suspended on the interior Graphite Powder 99 top of crucible in the described step 5.
The purity of described Si powder is 99.5%, and granularity is 300 orders.
The purity of described C powder is 99%, and granularity is 320 orders.
The purity of described SiC powder is 98.5%, and granularity is 300 orders.
Described Al
2O
3The purity of powder is analytical pure, and granularity is 100～200 orders.
The purity of described Graphite Powder 99 is 98%, and granularity is 400 orders.
Beneficial effect
The preparation method of a kind of overlong nanowire toughening ceramic coating that the present invention proposes, adopt the toughness reinforcing C/C composite material antioxidation of ultralong SiC nanowires ceramic coating, by himself larger length-to-diameter ratio can be effectively with the load transfer in the matrix to from it, and then the toughness of raising ceramic coating, reduce the cracking trend of ceramic coating, finally improve the anti-aging capability of ceramic coating.Compare with background technology, the toughness reinforcing ceramic coating of the ultralong SiC nanowires of preparation can be realized the effective protection against oxidation to the C/C matrix material.Result of study shows: coating specimens keeps the state of weightening finish always in the thermogravimetric process of the test of room temperature to 1500 ° C, and maximum rate of body weight gain is 1.21%～1.43%.
Compare with traditional nano wire, overlong nanowire is as toughness reinforcing phase time, by himself larger length-to-diameter ratio can be effectively with the load transfer in the matrix to from it, and then improve the toughness of ceramic coating, reduce the cracking trend of ceramic coating, improve the anti-aging capability of ceramic coating.
Description of drawings
Fig. 1 is the prepared ultralong SiC nanowires surface SEM photo of inventive embodiments 2;
Fig. 2 is the prepared toughness reinforcing ceramic coating section SEM photo of ultralong SiC nanowires of the embodiment of the invention 2;
Fig. 3 is that the prepared coating specimens of the embodiment of the invention 2 is in the thermogravimetric test-results of room temperature to 1500 ° C.
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Embodiment 1:
The sand paper that the C/C matrix material is used respectively No. 400, No. 800 and No. 1000 is clean with absolute ethanol washing behind the sanding and polishing successively, dry for standby in baking oven.
Take by weighing respectively the Si powder of 60g, the SiC powder of 15g, the C powder of 15g, the Al of 10g
2O
3Powder.Place ball grinder, get the agate ball of different quantities different diameter and put into ball grinder, carry out ball milling combination treatment 2h at planetary ball mill, obtain the embedding powder.
Above-mentioned 1/4 embedding powder is put into plumbago crucible, put into the C/C matrix material for preparing, put into again above-mentioned 1/4 embedding powder; make powder coat equably the C/C matrix material; then plumbago crucible is put into the pyroreaction sintering oven, afterwards furnace temperature is risen to 2200 ° of C, temperature rise rate is 10 ° of C/min; then be incubated 1h; powered-down naturally cools to room temperature subsequently, and crucible is taken out in logical Ar protection subsequently in the whole process; the cleaning powder obtains the C/C matrix material that ceramic coating coats.
Graphite Powder 99 is put into plumbago crucible, make its uniform spreading be placed on crucible bottom, the C/C matrix material that again ceramic coating that obtains is coated bundlees rear-mounted above Graphite Powder 99 with a branch of 3K carbon fiber, then plumbago crucible is put into the pyroreaction sintering oven, afterwards furnace temperature is risen to 1400 ° of C, temperature rise rate is 5 ° of C/min, then is incubated 3h.Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.Take out subsequently plumbago crucible, the carbon fiber of cleaning material surface obtains the surface with the C/C matrix material of the ceramic coating coating of ultralong SiC nanowires.
1/4 of above-mentioned embedding powder is put into plumbago crucible, put into the C/C matrix material that the surface for preparing coats with the ceramic coating of ultralong SiC nanowires, put into again 1/4 embedding powder, the slight crucible that rocks, make the embedding powder then plumbago crucible be put into the pyroreaction sintering oven with the C/C matrix material of the ceramic coating coating of ultralong SiC nanowires in the embedding surface equably, afterwards furnace temperature is risen to 2200 ° of C, temperature rise rate is 10 ° of C/min, then is incubated 1h.Powered-down naturally cools to room temperature subsequently, logical Ar protection in the whole process.Take out subsequently crucible, cleaning embedding powder obtains the C/C matrix material that ultralong SiC nanowires toughening ceramic coating coats.The result shows: coating specimens keeps the state of weightening finish always in the thermogravimetric process of the test of room temperature to 1500 ° C, and maximum rate of body weight gain is 1.21%.
Embodiment 2:
The sand paper that the C/C matrix material is used respectively No. 400, No. 800 and No. 1000 is clean with absolute ethanol washing behind the sanding and polishing successively, dry for standby in baking oven.
Take by weighing respectively the Si powder of 72g, the SiC powder of 10g, the C powder of 11g, the Al of 7g
2O
3Powder.Place ball grinder, get the agate ball of different quantities different diameter and put into ball grinder, carry out ball milling combination treatment 3h at planetary ball mill, obtain the embedding powder.
Above-mentioned 1/4 embedding powder is put into plumbago crucible, put into the C/C matrix material for preparing, put into again above-mentioned 1/4 embedding powder; make powder coat equably the C/C matrix material; then plumbago crucible is put into the pyroreaction sintering oven, afterwards furnace temperature is risen to 2100 ° of C, temperature rise rate is 7 ° of C/min; then be incubated 2h; powered-down naturally cools to room temperature subsequently, and crucible is taken out in logical Ar protection subsequently in the whole process; the cleaning powder obtains the C/C matrix material that ceramic coating coats.
Graphite Powder 99 is put into plumbago crucible, make its uniform spreading be placed on crucible bottom, the C/C matrix material that again ceramic coating that obtains is coated bundlees rear-mounted above Graphite Powder 99 with a branch of 3K carbon fiber, then plumbago crucible is put into the pyroreaction sintering oven, afterwards furnace temperature is risen to 1500 ° of C, temperature rise rate is 7 ° of C/min, then is incubated 2h.Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.Take out subsequently plumbago crucible, the carbon fiber of cleaning material surface obtains the surface with the C/C matrix material of the ceramic coating coating of ultralong SiC nanowires
1/4 of above-mentioned embedding powder is put into plumbago crucible, put into the C/C matrix material that the surface for preparing coats with the ceramic coating of ultralong SiC nanowires, put into again 1/4 embedding powder, the slight crucible that rocks, make the embedding powder then plumbago crucible be put into the pyroreaction sintering oven with the C/C matrix material of the ceramic coating coating of ultralong SiC nanowires in the embedding surface equably, afterwards furnace temperature is risen to 2100 ° of C, temperature rise rate is 7 ° of C/min, then is incubated 2h.Powered-down naturally cools to room temperature subsequently, logical Ar protection in the whole process.Take out subsequently crucible, cleaning embedding powder obtains the C/C matrix material with ultralong SiC nanowires toughening ceramic coating.As seen from Figure 1, the SiC nanowire length of preparation reaches several millimeters, and diameter Distribution is in 50～200nm scope, and these nano wires freely are orientated ground, are evenly distributed in ceramic surface.As seen from Figure 2, the nano wire of extracting that has a large amount of length on the section of ceramic coating.As shown in Figure 3, coating specimens keeps the state of weightening finish always in the thermogravimetric process of the test of room temperature to 1500 ° C, and maximum rate of body weight gain is 1.43%.
Embodiment 3
The sand paper that the C/C matrix material is used respectively No. 400, No. 800 and No. 1000 is clean with absolute ethanol washing behind the sanding and polishing successively, dry for standby in baking oven.
Take by weighing respectively the Si powder of 85g, the SiC powder of 5g, the C powder of 7g, the Al of 3g
2O
3Powder.Place ball grinder, get the agate ball of different quantities different diameter and put into ball grinder, carry out ball milling combination treatment 4h at planetary ball mill, obtain the embedding powder.
Above-mentioned 1/4 embedding powder is put into plumbago crucible, put into the C/C matrix material for preparing, put into again above-mentioned 1/4 embedding powder; make powder evenly coat the C/C matrix material; then plumbago crucible is put into the pyroreaction sintering oven, afterwards furnace temperature is risen to 2000 ° of C, temperature rise rate is 5 ° of C/min; then be incubated 2h; powered-down naturally cools to room temperature subsequently, and crucible is taken out in logical Ar protection subsequently in the whole process; the cleaning powder obtains the C/C matrix material that ceramic coating coats.
Graphite Powder 99 is put into plumbago crucible, make its uniform spreading be placed on crucible bottom, the C/C matrix material that again ceramic coating that obtains is coated bundlees rear-mounted above Graphite Powder 99 with a branch of 3K carbon fiber, then plumbago crucible is put into the pyroreaction sintering oven, afterwards furnace temperature is risen to 1600 ° of C, temperature rise rate is 10 ° of C/min, then is incubated 1h.Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.Take out subsequently plumbago crucible, the carbon fiber of cleaning material surface obtains the surface with the C/C matrix material of the ceramic coating coating of ultralong SiC nanowires.
Above-mentioned 1/4 embedding powder is put into plumbago crucible, put into the C/C matrix material that the surface for preparing coats with the ceramic coating of ultralong SiC nanowires, put into again 1/4 embedding powder, the slight crucible that rocks, make the embedding powder then plumbago crucible be put into the pyroreaction sintering oven with the C/C matrix material of the ceramic coating coating of ultralong SiC nanowires in the embedding surface equably, afterwards furnace temperature is risen to 2000 ° of C, temperature rise rate is 5 ° of C/min, then is incubated 3h.Powered-down naturally cools to room temperature subsequently, logical Ar protection in the whole process.Take out subsequently crucible, cleaning embedding powder obtains the C/C matrix material that ultralong SiC nanowires toughening ceramic coating coats.The result shows: coating specimens keeps the state of weightening finish always in the thermogravimetric process of the test of room temperature to 1500 ° C, and maximum rate of body weight gain is 1.36%.
Claims (8)
1. the preparation method of an overlong nanowire toughening ceramic coating is characterized in that step is as follows:
Step 1: with cleaning behind the C/C matrix material sanding and polishing, then put into baking oven and dry;
Step 2: take by weighing mass percent and be 60～85% Si powder, 5～15% SiC powder, 7～15% C powder and 3～10% Al
2O
3Powder places ball grinder, the powder that ball milling combination treatment 2～4h obtains mixing;
Step 3: the part powder is laid in the plumbago crucible, puts into again the C/C matrix material of oven dry, cover again on the C/C matrix material and establish the part powder;
Step 4: plumbago crucible is put into the pyroreaction sintering oven, with 5～10 ° of C/min heat-up rates furnace temperature is risen to 2000～2200 ° of C from room temperature, insulation 1～3h; Powered-down naturally cools to room temperature subsequently, and omnidistance Ar gas protection obtains the C/C matrix material with ceramic coating;
Step 5: Graphite Powder 99 is put into plumbago crucible, make its even bedding in crucible bottom, will bundle with the C/C matrix material of ceramic coating above the Graphite Powder 99 of rear-mounted in crucible again;
Step 6: plumbago crucible is put into the pyroreaction sintering oven, with 5～10 ° of C/min heat-up rates furnace temperature is risen to 1400～1600 ° of C from room temperature, insulation 1～3h; Powered-down naturally cools to room temperature subsequently, and logical Ar protection in the whole process obtains the surface with the C/C matrix material of the ceramic coating coating of ultralong SiC nanowires;
Step 7: the part powder of step 2 preparation is laid in the plumbago crucible, puts into again the C/C matrix material that the surface coats with the ceramic coating of ultralong SiC nanowires, again the cover part powder;
Step 8: plumbago crucible is put into the pyroreaction sintering oven, with 5～10 ° of C/min heat-up rates furnace temperature is risen to 2000～2200 ° of C from room temperature, insulation 1～3h; Powered-down naturally cools to room temperature subsequently, and logical argon shield obtains overlong nanowire toughening ceramic coating at the C/C composite material surface in the whole process.
2. the preparation method of described overlong nanowire toughening ceramic coating according to claim 1, it is characterized in that: the part powder in described step 3 and the step 7 is 1/4 of powder.
3. the preparation method of described overlong nanowire toughening ceramic coating according to claim 1 is characterized in that: adopt a branch of 3k carbon fiber binding C/C matrix material to be suspended on Graphite Powder 99 top in the crucible in the described step 5.
4. the preparation method of described overlong nanowire toughening ceramic coating according to claim 1, it is characterized in that: the purity of described Si powder is 99.5%, granularity is 300 orders.
5. the preparation method of described overlong nanowire toughening ceramic coating according to claim 1, it is characterized in that: the purity of described C powder is 99%, granularity is 320 orders.
6. the preparation method of described overlong nanowire toughening ceramic coating according to claim 1, it is characterized in that: the purity of described SiC powder is 98.5%, granularity is 300 orders.
7. the preparation method of described overlong nanowire toughening ceramic coating according to claim 1 is characterized in that: described Al
2O
3The purity of powder is analytical pure, and granularity is 100～200 orders.
8. the preparation method of described overlong nanowire toughening ceramic coating according to claim 1, it is characterized in that: the purity of described Graphite Powder 99 is 98%, granularity is 400 orders.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467126A (en) * | 2013-08-30 | 2013-12-25 | 西北工业大学 | Preparation method of SiC nanowire modified C/C composite material |
| CN105036801A (en) * | 2015-07-17 | 2015-11-11 | 常州大学 | Carbon/carbon composite material surface high temperature oxidation resistant coating and preparation method thereof |
| CN106866166A (en) * | 2017-03-20 | 2017-06-20 | 西北工业大学 | The method for improving carbon/carbon compound material and lithium aluminosilicate glass ceramic joining performance |
| CN108329056A (en) * | 2018-01-20 | 2018-07-27 | 南京航空航天大学 | A kind of method on reinforcement Continuous Fiber Reinforced Ceramic Matrix Composites surface |
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| CN101811892A (en) * | 2010-04-08 | 2010-08-25 | 西北工业大学 | Method for preparing nanowire-toughened carbon/carbon composite material ceramic coating |
| CN102701207A (en) * | 2012-06-21 | 2012-10-03 | 西北工业大学 | Method for preparing Al-doped silicon carbide nanowires |
| CN102745998A (en) * | 2012-06-21 | 2012-10-24 | 西北工业大学 | Preparation method for anti-oxidant silica-based ceramic coating with wide temperature range for carbon/carbon composite |
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| CN101811892A (en) * | 2010-04-08 | 2010-08-25 | 西北工业大学 | Method for preparing nanowire-toughened carbon/carbon composite material ceramic coating |
| CN102701207A (en) * | 2012-06-21 | 2012-10-03 | 西北工业大学 | Method for preparing Al-doped silicon carbide nanowires |
| CN102745998A (en) * | 2012-06-21 | 2012-10-24 | 西北工业大学 | Preparation method for anti-oxidant silica-based ceramic coating with wide temperature range for carbon/carbon composite |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103467126A (en) * | 2013-08-30 | 2013-12-25 | 西北工业大学 | Preparation method of SiC nanowire modified C/C composite material |
| CN103467126B (en) * | 2013-08-30 | 2014-08-20 | 西北工业大学 | Preparation method of SiC nanowire modified C/C composite material |
| CN105036801A (en) * | 2015-07-17 | 2015-11-11 | 常州大学 | Carbon/carbon composite material surface high temperature oxidation resistant coating and preparation method thereof |
| CN106866166A (en) * | 2017-03-20 | 2017-06-20 | 西北工业大学 | The method for improving carbon/carbon compound material and lithium aluminosilicate glass ceramic joining performance |
| CN108329056A (en) * | 2018-01-20 | 2018-07-27 | 南京航空航天大学 | A kind of method on reinforcement Continuous Fiber Reinforced Ceramic Matrix Composites surface |
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Application publication date: 20130501 |