CN107056303A - It is a kind of to prepare ZrB in zirconium aluminium carbon/carbon/silicon carbide composite material surface2The method of/SiC coatings - Google Patents
It is a kind of to prepare ZrB in zirconium aluminium carbon/carbon/silicon carbide composite material surface2The method of/SiC coatings Download PDFInfo
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- CN107056303A CN107056303A CN201710245487.3A CN201710245487A CN107056303A CN 107056303 A CN107056303 A CN 107056303A CN 201710245487 A CN201710245487 A CN 201710245487A CN 107056303 A CN107056303 A CN 107056303A
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 49
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 41
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 20
- RQMIWLMVTCKXAQ-UHFFFAOYSA-N [AlH3].[C] Chemical compound [AlH3].[C] RQMIWLMVTCKXAQ-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000000576 coating method Methods 0.000 title claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 title claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 8
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 8
- 239000011591 potassium Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000005498 polishing Methods 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims 1
- 229910001928 zirconium oxide Inorganic materials 0.000 claims 1
- 229910007948 ZrB2 Inorganic materials 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000011068 loading method Methods 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 description 14
- 238000007254 oxidation reaction Methods 0.000 description 14
- 239000000463 material Substances 0.000 description 5
- 230000003026 anti-oxygenic effect Effects 0.000 description 4
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 208000021017 Weight Gain Diseases 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 235000006708 antioxidants Nutrition 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000004584 weight gain Effects 0.000 description 3
- 235000019786 weight gain Nutrition 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011153 ceramic matrix composite Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000019612 pigmentation Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- -1 zirconium-aluminium-carbon Chemical compound 0.000 description 1
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
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Abstract
The invention belongs to high temperature coatings preparation field, the means for being related to a kind of utilization boronising prepare ZrB2The method of/SiC coatings.Described preparation method comprises the following steps：A, take the g of boron carbide 80 ~ 100, the g of carborundum 80 ~ 100 that granularity is 60 mesh, the g of potassium fluoborate 5 ~ 10 that granularity is 100 mesh that granularity is 200 mesh that they are placed in batch mixer by weight, using dry or wet mixing, after being sufficiently mixed, compound is made；B, compound obtained by step a is placed in drying box, 0.5 ~ 2h is dried under the conditions of 100 ~ 200 DEG C；C, block zirconium aluminium carbon/composite material of silicon carbide polishing by 4mm × 4mm × 4mm, it is embedded in using in dried compound obtained by step b and loading crucible, crucible is placed in high temperature furnace, under inert atmosphere conditions, it is heat-treated under conditions of 1300 ~ 1700 DEG C, 0.5 ~ 3h, compact structure, ZrB in uniform thickness is made2/ SiC figure layers.The features such as this method has simple production process, low production cost, it is easy to industrialized production.
Description
Technical field
The invention belongs to high temperature coatings preparation field, and in particular to a kind of means of utilization boronising prepare ZrB2/
The method of SiC coatings.
Background technology
Ternary layered ceramic Zr-Al-C be developed on the basis of ZrC can be as high temperature or superhigh temperature structure
The new ceramics that part is used, it has excellent room temperature and mechanical behavior under high temperature and good high temperature oxidation resistance.It is logical
Cross add the second phase SiC particulate prepared by zirconium aluminium carbon/composite material of silicon carbide have more excellent hardness, bending strength,
Fracture toughness and superhigh temperature (1600 DEG C of ＞) antioxygenic property.But SiC especially less than 1100 DEG C oxygen in lower temperature
The amount that the very slow therefore above-mentioned oxide containing silicon of change speed is produced at this temperature is less, is not enough to be formed the protection of densification
Film and play good protectiveness.Therefore zirconium aluminium carbon/composite material of silicon carbide is further improved anti-oxidant at 1000 DEG C or so
Performance is most important for the use of this material.
ZrB2/ SiC ceramic matrix composite material is most superhigh temperature ceramics systems of people's research in the last few years, and it has high hard
Degree, intensity, toughness and good conduction, thermal conductivity and chemical stability.In addition, ZrB2/ SiC composites compared with
All there is excellent antioxygenic property within the scope of wide temperature.One layer of continuous densification can be generated when being aoxidized when less than 1100 DEG C
Liquid phase B2O3Diaphragm, it effectively can prevent oxygen from inwardly spreading；Between 1100-1400 DEG C, although have part B2O3This
When start volatilization, but the B in this temperature range2O3Also there is certain protectiveness, in addition, SiC is opened in this temperature range
Originate raw oxidation, the SiO of generation2The inoxidizability of material can be improved；At more than 1400 DEG C, although most of B2O3Wave
Hair, but the oxide containing silicon of now SiC oxidations generation ensure that material still has preferable antioxygenic property.It is based on
ZrB2/ SiC ceramic matrix composite material the above plurality of advantages, it is all with a wide range of applications as high-temperature oxidation resistant coating.
In order to further improve the oxidation susceptibility of zirconium aluminium carbon/composite material of silicon carbide, it is necessary to explore a kind of low cost, work
Skill simply prepares anti-oxidant ZrB2The preparation method of/SiC coatings.
The content of the invention
It is an object of the invention to provide a kind of resistance to high temperature oxidation ZrB2The preparation method of/SiC coatings, further to change
The high temperature oxidation resistance of kind zirconium aluminium carbon/composite material of silicon carbide.This method has that technique is simple, the low feature of production cost.
The ZrB of the present invention2The preparation method of/SiC coatings comprises the following steps：
A, take by weight 80~100g of boron carbide, 80~100g of carborundum that granularity is 60 mesh that granularity is 200 mesh,
They are placed in batch mixer by granularity for 5~10g of potassium fluoborate of 100 mesh, using dry or wet mixing, after being sufficiently mixed, and are made
Compound；
B, compound obtained by step a is placed in drying box, 0.5~2h is dried under the conditions of 100~200 DEG C；
C, block zirconium aluminium carbon/composite material of silicon carbide polishing by 4mm × 4mm × 4mm, are embedded in and utilize step b institutes
In dried compound and load crucible, crucible is placed in high temperature furnace, under inert atmosphere conditions, 1300~
1700 DEG C, be heat-treated under conditions of 0.5~3h, compact structure, ZrB in uniform thickness is made2/ SiC figure layers.
Batch mixer of the present invention is in planetary ball mill, rotary mill, speed muller or high-speed mixer
Any one.
The decentralized medium that wet mixing of the present invention is used is any one in absolute ethyl alcohol or acetone.
High temperature furnace of the present invention is any one in carbon shirt-circuiting furnace, tube furnace or rotary furnace.
Inert atmosphere of the present invention is any one in argon gas or nitrogen.
Crucible of the present invention can be using alumina crucible or oxidation zirconium crucible.
The present invention is compared to the existing method for improving zirconium aluminium carbon/composite material of silicon carbide high temperature oxidation resistance, with as follows
Effect：
(1) present invention prepares silicide coating technique simply, by the mixture bag of boron carbide, carborundum and potassium fluoborate powder
Zirconium aluminium carbon/silicon carbide ceramics sample is buried, through high temperature thermal diffusion, antioxidant coating is obtained.Preparation process simultaneously is not required to apply external force, no
With carrying out in a vacuum, and it is with low cost.
(2) smooth surface can be handled using the present invention, moreover it is possible to practical work piece of the processing with complex surface, it is practical,
And once complete, production technology is simplified, it is easy to operate, it is adapted to industrialized production.
(3) because present invention utilizes ZrB2With SiC excellent antioxygenic property, so will be carried significantly using the present invention
The application of high zirconium-aluminium-carbon ceramic material
Brief description of the drawings
Fig. 1 is the X ray diffracting spectrum that figure layer is made using technique described in embodiment 1 for zirconium aluminium carbon/composite material of silicon carbide；
Fig. 2 is that the section Scanning Electron that figure layer is made using technique described in embodiment 1 in zirconium aluminium carbon/composite material of silicon carbide shows
Micro mirror photo；
Fig. 3 is the oxidation weight gain curve using zirconium aluminium carbon/composite material of silicon carbide before and after process modification described in embodiment 1
Figure；
5. embodiment
The present invention is further described below with reference to embodiment：
Embodiment 1：
It is 100 purposes to take boron carbide 80g, the carborundum 80g that granularity is 60 mesh, granularity that granularity is 200 mesh by weight
Potassium fluoborate 10g, they are placed in batch mixer, after being sufficiently mixed using dry pigmentation, and compound is made.Gained compound is put
In drying box, 1h is dried under the conditions of 150 DEG C.4mm × 4mm × 4mm block zirconium aluminium carbon/composite material of silicon carbide is thrown
Light processing, is embedded in compound and loads crucible, crucible is placed in high temperature furnace, at 1300 DEG C under the conditions of argon gas atmosphere
3h is incubated, ZrB is made2/ SiC figure layers (as shown in Figure 1).About 20 μm or so (such as Fig. 2 of manufactured coating compact structure, thickness
It is shown).
Embodiment 2：
It is 100 purposes to take boron carbide 100g, the carborundum 80g that granularity is 60 mesh, granularity that granularity is 200 mesh by weight
Potassium fluoborate 8g, they are placed in batch mixer, after being sufficiently mixed using dry pigmentation, and compound is made.Gained compound is put
In drying box, 0.5h is dried under the conditions of 200 DEG C.By 4mm × 4mm × 4mm block zirconium aluminium carbon/composite material of silicon carbide
Polishing, is embedded in compound and loads crucible, crucible is placed in high temperature furnace, 1500 under the conditions of argon gas atmosphere
DEG C insulation 2h, be made compact structure, the uniform ZrB of 30 μm of thickness2/ SiC figure layers.
Embodiment 3：
It is 100 purposes to take boron carbide 80g, the carborundum 100g that granularity is 60 mesh, granularity that granularity is 200 mesh by weight
Potassium fluoborate 5g, they are placed in batch mixer, after being sufficiently mixed using wet mixing method, and compound is made.Gained compound is put
In drying box, 2h is dried under the conditions of 100 DEG C.4mm × 4mm × 4mm block zirconium aluminium carbon/composite material of silicon carbide is thrown
Light processing, is embedded in compound and loads crucible, crucible is placed in high temperature furnace, at 1700 DEG C under the conditions of argon gas atmosphere
0.5h is incubated, compact structure, the uniform ZrB of 23 μm of thickness is made2/ SiC figure layers.
Comparative example：
It is 100 mesh to take boron carbide 160g, the carborundum 160g that granularity is 60 mesh, granularity that granularity is 200 mesh by weight
Potassium fluoborate 20g, compound is made according to embodiment 1 in they.By 4mm × 4mm × 4mm block zirconium aluminium carbon/carborundum
Composite polishing, uniform ZrB is made according to technique described by embodiment 12/ SiC figure layers.Sample before and after boronising is entered
The experiment of 1000 DEG C of constant temperature oxidations of row finds that sample 1000 DEG C of oxidations, 8 hours oxidation weight gains of non-boronisings reach 70 grams/m, and
It is only 28 grams/m by oxidation weight gain under the sample similarity condition of Bononizing pretreatment, the oxidisability of the sample after Bononizing pretreatment
Larger improvement (as shown in Figure 3) can have been obtained.
Claims (6)
1. a kind of prepare ZrB in zirconium aluminium carbon/carbon/silicon carbide composite material surface2The method of/SiC coatings, it is characterised in that：The side
Method comprises the following steps：
A, the g of boron carbide 80 ~ 100, the g of carborundum 80 ~ 100 that granularity is 60 mesh, granularity that granularity is 200 mesh is taken to be by weight
They are placed in batch mixer by the g of potassium fluoborate 5 ~ 10 of 100 mesh, using dry or wet mixing, after being sufficiently mixed, and compound is made；
B, compound obtained by step a is placed in drying box, 0.5 ~ 2h is dried under the conditions of 100 ~ 200 DEG C；
C, block zirconium aluminium carbon/composite material of silicon carbide polishing by 4mm × 4mm × 4mm, are embedded in using dry obtained by step b
In compound after dry and load crucible, crucible is placed in high temperature furnace, under inert atmosphere conditions, 1300 ~ 1700
DEG C, be heat-treated under conditions of 0.5 ~ 3h, compact structure, ZrB in uniform thickness is made2/ SiC figure layers.
2. preparation method according to claim 1, it is characterised in that：The batch mixer is planetary ball mill, roller ball
Any one in grinding machine, speed muller or high-speed mixer.
3. preparation method according to claim 1, it is characterised in that：The decentralized medium that the wet mixing is used is absolute ethyl alcohol
Or any one in acetone.
4. preparation method according to claim 1, it is characterised in that：The high temperature furnace be carbon shirt-circuiting furnace, tube furnace or
Any one in rotary furnace.
5. preparation method according to claim 1, it is characterised in that：The inert atmosphere is any in argon gas or nitrogen
It is a kind of.
6. preparation method according to claim 1, it is characterised in that：The crucible can use alumina crucible or zirconium oxide
Crucible.
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| CN111334743A (en) * | 2020-03-15 | 2020-06-26 | 河北工业大学 | Preparation method of zirconium boride-zirconium carbide-silicon carbide composite coating |
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