CN103819227A - Preparation method of ZrB2-SiC/SiC ceramic coating - Google Patents

Preparation method of ZrB2-SiC/SiC ceramic coating Download PDF

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CN103819227A
CN103819227A CN201410001380.0A CN201410001380A CN103819227A CN 103819227 A CN103819227 A CN 103819227A CN 201410001380 A CN201410001380 A CN 201410001380A CN 103819227 A CN103819227 A CN 103819227A
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powder
sic
massfraction
zrb
raw material
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CN103819227B (en
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张幸红
韩文波
王鹏
洪长青
胡平
张兆停
熊漫漫
王公平
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention relates to a preparation method of a ceramic coating, in particular to a preparation method of a ZrB2-SiC/SiC ceramic coating. The method aims at solving the technical problem that a silica-based ceramic coating on the surfaces of the existing graphite material, the C/C composite and the C/SiC composite is poor in oxidation resistance. The preparation method employs an embedding method and comprises the steps of: 1, preparing an intermediate layer SiC, and 2, preparing the ZrB2-SiC/SiC ceramic coating. The prepared ceramic coating is strong in oxidation resistance. The method is mainly applied to the field of preparing the zirconium boride based ceramic coating.

Description

A kind of ZrB 2the preparation method of-SiC/SiC ceramic coating
Technical field
The present invention relates to a kind of preparation method of ceramic coating.
Background technology
Anti-oxidant problem is the subject matter that limits its use that the high-temperature structural materials such as graphite material, C/C matrix material and C/SiC matrix material exist always, and preparing multiphase ceramic coating on its surface is a kind of effective ways that solve the anti-oxidant problem of this class material.
SiC due to its moderate thermal expansivity and and graphite material, C/C matrix material and ceramic coating between good physical and chemical compatibility, be a kind of good key coat material, and after silicon-based ceramic material oxidation, can form the SiO of the even compact that at high temperature oxygen diffusion rate is low 2glass coating, for body material provides good anti-oxidation protection performance.But, along with the rising of temperature and the prolongation of oxidization time, SiO 2in glass coating, can form cavity and bubble, for oxygen provides passage to the diffusion of body material, and single SiO 2glassy phase in use can slowly volatilize, and causes the consumption gradually of coated material.
ZrB 2stupalith has oxidation-resistance good under high-melting-point, high strength and high temperature, is a kind of material in aerospace field with applications well prospect.ZrB 2the ZrO that oxidation forms 2can with SiO 2reaction forms ZrSiO 4, ZrSiO 4there is good high-temperature oxidation resistance, can at 1973K temperature, use for a long time.The ZrSiO of high thermal stability 4be present in mutually SiO 2in layer, can reduce SiO 2consumption and improve the oxidation-resistance of SiC coating, and due to ZrB 2the B that oxidation forms at low temperatures 2o 3stickiness very low, more than 1373K volatilization serious, also make ZrB 2material can not be served as single coated material and be used.And at ZrB 2in material, add silicon based material, as SiC, ZrC, HfC etc. can form borosilicate glass phase after oxidation, improve anti-ablation and the antioxidant property of material.Due to ZrB 2with the special performance that SiC is used in conjunction with, ZrB 2-SiC stupalith has been seen as one of very promising stupalith can be used in extreme environment.
Summary of the invention
The present invention is the poor technical problem of silicon based ceramic coating antioxidant property that will solve current graphite material, C/C matrix material and C/SiC composite material surface, thereby a kind of ZrB is provided 2the preparation method of-SiC/SiC ceramic coating.
A kind of ZrB of the present invention 2the preparation method of-SiC/SiC ceramic coating carries out according to the following steps:
One, the preparation of middle layer SiC: Si powder and C powder are evenly mixed, obtain raw material 1; Si powder, C powder and SiC powder are evenly mixed, obtain raw material 2; By B 2o 3, Al 2o 3, a kind of in ferrocene and nickelocene or several mixture wherein, obtain additive 1; Additive 1 is dry in rotatory evaporator after wet mixing ball milling mixes with raw material 1 or raw material 2, obtain powder mix 1; With sand paper by base member to be coated polishing chamfering, adopt entrapping method that the base member to be coated of having polished is embedded in powder mix 1, obtain the base member of embedding powder mix 1, then the base member of embedding powder mix 1 being heated to temperature under vacuum or protective atmosphere is 1400 ℃～2200 ℃, and be to be incubated 10min～4h under the condition of 1400 ℃～2200 ℃ in temperature, cool to room temperature with the furnace, then, after ultrasonic cleaning and being dried, obtain the base member of embedding middle layer SiC; The massfraction of the additive 1 in the powder mix 1 described in step 1 is 0～18%; In raw material 1 described in step 1, the massfraction of Si powder is that the massfraction of 30%～85%, C powder is 15%～70%; The massfraction that in raw material 2 described in step 1, the massfraction of Si powder is 20%～80%, the massfraction of C powder is 2%～20%, SiC powder is that the massfraction summation of 3%～60%, Si powder, C powder and SiC powder is 100%;
Two, ZrB 2the preparation of-SiC/SiC ceramic coating: by ZrB 2powder, Si powder and C powder evenly mix, and obtain raw material 3; B powder, Zr powder and SiC powder are evenly mixed, obtain raw material 4; By ZrB 2powder, Si powder, C powder and SiC powder evenly mix, and obtain raw material 5; By B powder, Zr powder, SiC powder and ZrB 2powder evenly mixes, and obtains raw material 6; By ZrB 2powder, Si powder, C powder, SiC powder and B powder evenly mix, and obtain raw material 7; By ZrB 2powder, Si powder, C powder, SiC powder and Zr powder evenly mix, and obtain raw material 8; By B powder, Zr powder, SiC powder, ZrB 2powder and Si powder evenly mix, and obtain raw material 9; By ZrB 2powder, B powder, Zr powder, Si powder, C powder and SiC powder evenly mix, and obtain raw material 10; By SiO 2, B 2o 3, Al 2o 3, a kind of in ferrocene and nickelocene or several mixture wherein, obtain additive 2; Additive 2 is dry in rotatory evaporator after wet mixing ball milling mixes with raw material 3, raw material 4, raw material 5, raw material 6, raw material 7, raw material 8, raw material 9 or raw material 10, obtain powder mix 2; The base member of the embedding middle layer SiC that employing entrapping method obtains step 1 is embedded in powder mix 2; obtain the base member of embedding powder mix 2; then the base member of embedding powder mix 2 being heated to temperature under vacuum or protective atmosphere is 1400 ℃～3600 ℃; and be to be incubated 10min～6h under the condition of 1400 ℃～3600 ℃ in temperature; cool to room temperature with the furnace, obtain ZrB 2-SiC/SiC ceramic coating; The massfraction of the additive 2 in the powder mix 2 described in step 2 is 0～18%; ZrB in raw material 3 described in step 2 2the massfraction of powder is 50%～80%, the massfraction of Si powder is 3%～80%, the massfraction of C powder is 2%～20%, ZrB 2the massfraction summation of powder, Si powder and C powder is 100%; The massfraction summation that in raw material 4 described in step 2, the massfraction of B powder is 20%～50%, the massfraction of Zr powder is 10%～50%, the massfraction of SiC powder is 3%～50%, B powder, Zr powder and SiC powder is 100%; ZrB in raw material 5 described in step 2 2the massfraction of powder is 50%～80%, the massfraction of Si powder is 3%～80%, the massfraction of C powder is 2%～20%, the massfraction of SiC powder is 3%～50%, ZrB 2the massfraction summation of powder, Si powder, C powder and SiC powder is 100%; In raw material 6 described in step 2, B powder massfraction is 20%～50%, Zr powder massfraction is 10%～50%, SiC powder massfraction is 3%～50%, ZrB 2powder massfraction is 50%～80%, B powder, Zr powder, SiC powder and ZrB 2the massfraction summation of powder is 100%; ZrB in raw material 7 described in step 2 2powder massfraction is 50%～80%, Si powder massfraction is 3%～80%, C powder massfraction is 2%～20%, SiC powder massfraction is 3%～50%, B powder massfraction is 20%～50%, ZrB 2the massfraction summation of powder, Si powder, C powder, SiC powder and B powder is 100%; ZrB in raw material 8 described in step 2 2powder massfraction is 50%～80%, Si powder massfraction is 3%～80%, C powder massfraction is 2%～20%, SiC powder massfraction is 3%～50%, Zr powder massfraction is 10%～50%, ZrB 2the massfraction summation of powder, Si powder, C powder, SiC powder and Zr powder is 100%; In raw material 9 described in step 2, B powder massfraction is 20%～50%, Zr powder massfraction is 10%～50%, SiC powder massfraction is 3%～50%, ZrB 2powder massfraction is 50%～80%, Si powder massfraction is 3%～80%, B powder, Zr powder, SiC powder, ZrB 2the massfraction summation of powder and Si powder is 100%; ZrB in raw material 10 described in step 2 2powder massfraction is 50%～80%, B powder massfraction is 20%～50%, Zr powder massfraction is 10%～50%, Si powder massfraction is 3%～80%, C powder massfraction is 2%～20%, SiC powder massfraction is 3%～50%, ZrB 2the massfraction summation of powder, B powder, Zr powder, Si powder, C powder and SiC powder is 100%.
Advantage of the present invention:
One, of the present invention have a bi-layer coating structure, makes more than matrix uses 200h in the high temperature oxidation stability atmosphere of 1500 ℃;
Two, the present invention can obtain by the ratio of each raw material in change entrapping method coating and preparation technology the SiC/(ZrB of different tissues structure and thickness 2-SiC) coating, can meet different requirements.
Accompanying drawing explanation
Fig. 1 is ZrB of the present invention 2the schematic diagram of-SiC/SiC ceramic coating, 1 is outer coating ZrB 2-SiC, 2 is middle layer SiC, 3 is base member;
Fig. 2 tests the electron scanning micrograph of the middle layer SiC coating that in, step 1 obtains;
Fig. 3 tests the outer coating ZrB that in, step 2 obtains 2the scanning electron photomicrograph of-SiC;
The test data curve that Fig. 4 obtains for test two, curve 1 is figure of merit curve, curve 2 is rate of weight loss curve;
Fig. 5 is the electron scanning micrograph of the middle layer SiC coating that in test three, step 1 obtains;
Fig. 6 tests the ZrB that three step 2 obtain 2the scanning electron photomicrograph of-SiC outer coating;
The test data curve that Fig. 7 obtains for test four, curve 1 is figure of merit curve, curve 2 is rate of weight loss curve;
Fig. 8 is the electron scanning micrograph of the middle layer SiC coating that in test five, step 1 obtains;
Fig. 9 is the ZrB obtaining in test five 2the scanning electron photomicrograph of-SiC outer coating;
The test data curve that Figure 10 obtains for test six, curve 1 is figure of merit curve, curve 2 is rate of weight loss curve;
Figure 11 is test seven ZrB that obtain 2the scanning electron photomicrograph of-SiC outer coating;
The test data curve that Figure 12 obtains for test six, curve 1 is figure of merit curve, curve 2 is rate of weight loss curve.
Embodiment
Embodiment one: a kind of ZrB in present embodiment 2the preparation method of-SiC/SiC ceramic coating carries out according to the following steps:
One, the preparation of middle layer SiC: Si powder and C powder are evenly mixed, obtain raw material 1; Si powder, C powder and SiC powder are evenly mixed, obtain raw material 2; By B 2o 3, Al 2o 3, a kind of in ferrocene and nickelocene or several mixture wherein, obtain additive 1; Additive 1 is dry in rotatory evaporator after wet mixing ball milling mixes with raw material 1 or raw material 2, obtain powder mix 1; With sand paper by base member to be coated polishing chamfering, adopt entrapping method that the base member to be coated of having polished is embedded in powder mix 1, obtain the base member of embedding powder mix 1, then the base member of embedding powder mix 1 being heated to temperature under vacuum or protective atmosphere is 1400 ℃～2200 ℃, and be to be incubated 10min～4h under the condition of 1400 ℃～2200 ℃ in temperature, cool to room temperature with the furnace, then, after ultrasonic cleaning and being dried, obtain the base member of embedding middle layer SiC; The massfraction of the additive 1 in the powder mix 1 described in step 1 is 0～18%; In raw material 1 described in step 1, the massfraction of Si powder is that the massfraction of 30%～85%, C powder is 15%～70%; The massfraction that in raw material 2 described in step 1, the massfraction of Si powder is 20%～80%, the massfraction of C powder is 2%～20%, SiC powder is that the massfraction summation of 3%～60%, Si powder, C powder and SiC powder is 100%;
Two, ZrB 2the preparation of-SiC/SiC ceramic coating: by ZrB 2powder, Si powder and C powder evenly mix, and obtain raw material 3; B powder, Zr powder and SiC powder are evenly mixed, obtain raw material 4; By ZrB 2powder, Si powder, C powder and SiC powder evenly mix, and obtain raw material 5; By B powder, Zr powder, SiC powder and ZrB 2powder evenly mixes, and obtains raw material 6; By ZrB 2powder, Si powder, C powder, SiC powder and B powder evenly mix, and obtain raw material 7; By ZrB 2powder, Si powder, C powder, SiC powder and Zr powder evenly mix, and obtain raw material 8; By B powder, Zr powder, SiC powder, ZrB 2powder and Si powder evenly mix, and obtain raw material 9; By ZrB 2powder, B powder, Zr powder, Si powder, C powder and SiC powder evenly mix, and obtain raw material 10; By SiO 2, B 2o 3, Al 2o 3, a kind of in ferrocene and nickelocene or several mixture wherein, obtain additive 2; Additive 2 is dry in rotatory evaporator after wet mixing ball milling mixes with raw material 3, raw material 4, raw material 5, raw material 6, raw material 7, raw material 8, raw material 9 or raw material 10, obtain powder mix 2; The base member of the embedding middle layer SiC that employing entrapping method obtains step 1 is embedded in powder mix 2; obtain the base member of embedding powder mix 2; then the base member of embedding powder mix 2 being heated to temperature under vacuum or protective atmosphere is 1400 ℃～3600 ℃; and be to be incubated 10min～6h under the condition of 1400 ℃～3600 ℃ in temperature; cool to room temperature with the furnace, obtain ZrB 2-SiC/SiC ceramic coating; The massfraction of the additive 2 in the powder mix 2 described in step 2 is 0～18%; ZrB in raw material 3 described in step 2 2the massfraction of powder is 50%～80%, the massfraction of Si powder is 3%～80%, the massfraction of C powder is 2%～20%, ZrB 2the massfraction summation of powder, Si powder and C powder is 100%; The massfraction summation that in raw material 4 described in step 2, the massfraction of B powder is 20%～50%, the massfraction of Zr powder is 10%～50%, the massfraction of SiC powder is 3%～50%, B powder, Zr powder and SiC powder is 100%; ZrB in raw material 5 described in step 2 2the massfraction of powder is 50%～80%, the massfraction of Si powder is 3%～80%, the massfraction of C powder is 2%～20%, the massfraction of SiC powder is 3%～50%, ZrB 2the massfraction summation of powder, Si powder, C powder and SiC powder is 100%; In raw material 6 described in step 2, B powder massfraction is 20%～50%, Zr powder massfraction is 10%～50%, SiC powder massfraction is 3%～50%, ZrB 2powder massfraction is 50%～80%, B powder, Zr powder, SiC powder and ZrB 2the massfraction summation of powder is 100%; ZrB in raw material 7 described in step 2 2powder massfraction is 50%～80%, Si powder massfraction is 3%～80%, C powder massfraction is 2%～20%, SiC powder massfraction is 3%～50%, B powder massfraction is 20%～50%, ZrB 2the massfraction summation of powder, Si powder, C powder, SiC powder and B powder is 100%; ZrB in raw material 8 described in step 2 2powder massfraction is 50%～80%, Si powder massfraction is 3%～80%, C powder massfraction is 2%～20%, SiC powder massfraction is 3%～50%, Zr powder massfraction is 10%～50%, ZrB 2the massfraction summation of powder, Si powder, C powder, SiC powder and Zr powder is 100%; In raw material 9 described in step 2, B powder massfraction is 20%～50%, Zr powder massfraction is 10%～50%, SiC powder massfraction is 3%～50%, ZrB 2powder massfraction is 50%～80%, Si powder massfraction is 3%～80%, B powder, Zr powder, SiC powder, ZrB 2the massfraction summation of powder and Si powder is 100%; ZrB in raw material 10 described in step 2 2powder massfraction is 50%～80%, B powder massfraction is 20%～50%, Zr powder massfraction is 10%～50%, Si powder massfraction is 3%～80%, C powder massfraction is 2%～20%, SiC powder massfraction is 3%～50%, ZrB 2the massfraction summation of powder, B powder, Zr powder, Si powder, C powder and SiC powder is 100%.
In the time that the additive 1 described in present embodiment step 1 is mixture, in mixture, each component is mixed by any ratio and forms.
In the time that the additive 2 described in present embodiment step 2 is mixture, in mixture, each component is mixed by any ratio and forms.
The advantage of present embodiment:
One, present embodiment has a bi-layer coating structure, makes more than matrix uses 200h in the high temperature oxidation stability atmosphere of 1500 ℃;
Two, present embodiment can obtain by the ratio of each raw material in change entrapping method coating and preparation technology the SiC/(ZrB of different tissues structure and thickness 2-SiC) coating, can meet different requirements.
Embodiment two: present embodiment is different from embodiment one: the protection gas described in step 1 is argon gas or nitrogen, the vacuum tightness described in step 1 is below 100Pa.Other are identical with embodiment one.
Embodiment three: present embodiment is different from one of embodiment one or two: the base member of embedding powder mix being heated to temperature under protective atmosphere in step 1 is 1600 ℃～2000 ℃; and be to be incubated 1h～2h under the condition of 1600 ℃～2000 ℃ in temperature, cool to room temperature with the furnace.Other are identical with one of embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three: the batch mixing medium of the wet mixing ball milling described in step 1 and step 2 is alcohol.Other are identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four: all C powder described in step 1 and step 2 are graphite or carbon black.Other is identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five: the protection gas described in step 2 is argon gas or nitrogen, the vacuum tightness described in step 2 is below 100Pa.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six: the base member to be coated described in step 1 is graphite, C/C matrix material or C/SiC matrix material.Other is identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven: the base member of embedding powder mix 2 being heated to temperature under protective atmosphere in step 2 is 2000 ℃～3000 ℃; and be to be incubated 2h～4h under the condition of 2000 ℃～3000 ℃ in temperature; cool to room temperature with the furnace, obtain ZrB 2-SiC/SiC ceramic coating.Other is identical with one of embodiment one to seven.
Adopt following verification experimental verification effect of the present invention:
Test one: the ZrB of this test 2the preparation method of-SiC/SiC ceramic coating carries out according to the following steps:
One, the preparation of middle layer SiC: Si powder and Graphite Powder 99 are evenly mixed, obtain raw material 1; By Al 2o 3as additive 1; Additive 1 is dry in rotatory evaporator after wet mixing ball milling mixes with raw material 1, obtain powder mix 1; With 600 object sand paper by base member to be coated polishing chamfering, adopt entrapping method that the base member to be coated of having polished is embedded in powder mix 1, obtain the base member of embedding powder mix 1, then under the condition that is 80Pa in vacuum tightness, the base member of embedding powder mix 1 being heated to temperature is 1800 ℃, and be to be incubated 2h under the condition of 1800 ℃ in temperature, cool to room temperature with the furnace, then, after ultrasonic cleaning and being dried, obtain the base member of embedding middle layer SiC; The massfraction of the additive 1 in the powder mix 1 described in step 1 is 15%; In raw material 1 described in step 1, the massfraction of Si powder is 82.4%, and the massfraction of Graphite Powder 99 is 17.6%;
Two, ZrB 2the preparation of-SiC/SiC ceramic coating: by ZrB 2powder, Si powder and Graphite Powder 99 evenly mix, and obtain raw material 3; Raw material 3 is dry in rotatory evaporator after wet mixing ball milling mixes, obtain powder mix 2; The base member of the embedding middle layer SiC that employing entrapping method obtains step 1 is embedded in powder mix 2, obtain the base member of embedding powder mix 2, then under the condition that is 80Pa in vacuum tightness, the base member of embedding powder mix 2 being heated to temperature is 2200 ℃, and be to be incubated 2h under the condition of 2200 ℃ in temperature, cool to room temperature with the furnace, obtain ZrB 2-SiC/SiC ceramic coating; ZrB in raw material 3 described in step 2 2the massfraction of powder is 65%, the massfraction of Si powder is 28%, the massfraction of Graphite Powder 99 is 7%; The batch mixing medium of the wet mixing ball milling described in step 1 and step 2 is alcohol; Base member to be coated described in step 1 is graphite.
Fig. 2 tests the electron scanning micrograph of the middle layer SiC coating that in, step 1 obtains, and can find out that by this photo SiC middle layer has higher density, and coating flawless is conducive to improve the oxidation-resistance of Bulk coat; Because SiC middle layer quality is good, also help and the combination of outer coating, guarantee the quality of Bulk coat.
Fig. 3 tests the outer coating ZrB that in, step 2 obtains 2the scanning electron photomicrograph of-SiC, can find out ZrB by this photo 2-SiC outer coating has higher density, coatingsurface flawless, and this explanation coating can effectively hinder the diffusion of oxygen to matrix, and coating has good antioxidant property.
Test two: by test one ZrB obtaining 2-SiC/SiC ceramic coating carries out anti-oxidant test: by test one ZrB obtaining 2it is in the retort furnace of 1500 ℃ that-SiC/SiC ceramic coating is put into temperature, after insulation 30min, takes out, and at room temperature after cooling 30min, weighs, and repeats above-mentioned steps 15 times.
The test data curve that Fig. 4 obtains for test two, curve 1 is figure of merit curve, curve 2 is rate of weight loss curve, as can be seen from the figure sample is at the weightless 0.237g of sample after 15 loop tests, rate of weight loss is 26.3%, this is the destruction that has caused figure layer due to sample in the high low temperature test process of circulation due to the thermal stresses constantly producing, constantly produce oxygen and enter the passage of matrix, cause the continuous oxidation of matrix to cause, in the past the experiment situation of 5 times shows, through 5 circulation experiments, sample is weightless 0.021g only, rate of weight loss is only 1.9%, this illustrates that this coating does not have good antioxidant property in destruction situation, and the high Low Temperature Thermal that coating can be born certain number of times impacts and does not destroy, thereby the ZrB obtaining in test one is described 2-SiC/SiC ceramic coating has good antioxidant property, can effectively improve the oxidation-resistance of body material.
Test three: a kind of ZrB of this test 2the preparation method of-SiC/SiC ceramic coating carries out according to the following steps:
One, the preparation of middle layer SiC: Si powder and Graphite Powder 99 are evenly mixed, obtain raw material 1; By Al 2o 3mix in any proportion with ferrocene, obtain additive 1; Additive 1 is dry in rotatory evaporator after wet mixing ball milling mixes with raw material 1, obtain powder mix 1; With sand paper by base member to be coated polishing chamfering, adopt entrapping method that the base member to be coated of having polished is embedded in powder mix 1, obtain the base member of embedding powder mix 1, then under the condition that is 80Pa in vacuum tightness, the base member of embedding powder mix 1 being heated to temperature is 1900 ℃, and be to be incubated 2h under the condition of 1900 ℃ in temperature, cool to room temperature with the furnace, then, after ultrasonic cleaning and being dried, obtain the base member of embedding middle layer SiC; The massfraction of the additive 1 in the powder mix 1 described in step 1 is 17.9%; In raw material 1 described in step 1, the massfraction of Si powder is 83.3%, and the massfraction of Graphite Powder 99 is 16.7%;
Two, ZrB 2the preparation of-SiC/SiC ceramic coating: by ZrB 2powder, Si powder and C powder evenly mix, and obtain raw material 3; By B 2o 3as additive 2; Additive 2 is dry in rotatory evaporator after wet mixing ball milling mixes with raw material 3, obtain powder mix 2; The base member of the embedding middle layer SiC that employing entrapping method obtains step 1 is embedded in powder mix 2, obtain the base member of embedding powder mix 2, then under the condition that is 80Pa in vacuum tightness, the base member of embedding powder mix 2 being heated to temperature is 1900 ℃, and be to be incubated 2h under the condition of 1900 ℃ in temperature, cool to room temperature with the furnace, obtain ZrB 2-SiC/SiC ceramic coating; ZrB in raw material 3 described in step 2 2the massfraction of powder is 82.4%, the massfraction of Si powder is 12.4%, the massfraction of C powder is 5.2%; The massfraction of the additive 2 in the powder mix 2 described in step 2 is 1%; The batch mixing medium of the wet mixing ball milling described in step 1 and step 2 is alcohol; Base member to be coated described in step 1 is graphite.
Fig. 5 is the electron scanning micrograph of the middle layer SiC coating that obtains of step 1 in test three, can find out that by this photo SiC middle layer has higher density, and coating flawless is conducive to improve the oxidation-resistance of Bulk coat; Because SiC middle layer quality is good, also help and the combination of outer coating, guarantee the quality of Bulk coat.
Fig. 6 tests the ZrB that three step 2 obtain 2the scanning electron photomicrograph of-SiC outer coating, can find out ZrB by this photo 2it is not high that-SiC outer coating has density, and surface tissue is loose, and coating has and comes off, and this antioxidant effect that this coating is described is not as test one.
Test four: by test three ZrB that obtain 2-SiC/SiC ceramic coating carries out anti-oxidant test: by test three ZrB that obtain 2it is in the retort furnace of 1500 ℃ that-SiC/SiC ceramic coating is put into temperature, after insulation 30min, takes out, and at room temperature after cooling 30min, weighs, and repeats above-mentioned steps 15 times.
The test data curve that Fig. 7 obtains for test four, curve 1 is figure of merit curve, curve 2 is rate of weight loss curve, as can be seen from the figure sample exceedes 70% at sample rate of weight loss after 15 loop tests, this is because the density of sample own is not high, coatingsurface has a large amount of spaces to exist, and the continuous destruction that has caused figure layer in the high low temperature test process of circulation due to the thermal stresses constantly producing, constantly produce oxygen and enter the passage of matrix, cause the continuous oxidation of matrix to cause, because the matrix oxidation in oxidation test process of this coating is serious, coating could not reach effectively protects body material, antioxidant effect is not obvious.
Test five: a kind of ZrB of this test 2the preparation method of-SiC/SiC ceramic coating carries out according to the following steps:
One, the preparation of middle layer SiC: Si powder and Graphite Powder 99 are evenly mixed, obtain raw material 1; Raw material 1 is dry in rotatory evaporator after wet mixing ball milling mixes, obtain powder mix 1; With sand paper by base member to be coated polishing chamfering, adopt entrapping method that the base member to be coated of having polished is embedded in powder mix 1, obtain the base member of embedding powder mix 1, then under the condition that is 80Pa in vacuum tightness, the base member of embedding powder mix 1 being heated to temperature is 1800 ℃, and be to be incubated 2h under the condition of 1800 ℃ in temperature, cool to room temperature with the furnace, then, after ultrasonic cleaning and being dried, obtain the base member of embedding middle layer SiC; In raw material 1 described in step 1, the massfraction of Si powder is 82%, and the massfraction of Graphite Powder 99 is 18%;
Two, ZrB 2the preparation of-SiC/SiC ceramic coating: by ZrB 2powder, Si powder and C powder evenly mix, and obtain raw material 3; Raw material 3 is dry in rotatory evaporator after wet mixing ball milling mixes, obtain powder mix 2; The base member of the embedding middle layer SiC that employing entrapping method obtains step 1 is embedded in powder mix 2, obtain the base member of embedding powder mix 2, then under the condition that is 80Pa in vacuum tightness, the base member of embedding powder mix 2 being heated to temperature is 2200 ℃, and be to be incubated 2h under the condition of 2200 ℃ in temperature, cool to room temperature with the furnace, obtain ZrB 2-SiC/SiC ceramic coating; ZrB in raw material 3 described in step 2 2the massfraction of powder is 62%, the massfraction of Si powder is 31%, the massfraction of Graphite Powder 99 is 7%; The batch mixing medium of the wet mixing ball milling described in step 1 and step 2 is alcohol; Base member to be coated described in step 1 is graphite.
Fig. 8 is the electron scanning micrograph of the middle layer SiC coating that obtains of step 1 in test five, can find out that by this photo SiC middle layer has higher density, and coating flawless is conducive to improve the oxidation-resistance of Bulk coat; Because SiC middle layer quality is good, also help and the combination of outer coating, guarantee the quality of Bulk coat.
Fig. 9 is the ZrB obtaining in test five 2the scanning electron photomicrograph of-SiC outer coating, can find out ZrB by this photo 2-SiC outer coating has very high density, coatingsurface flawless, and this explanation coating can effectively hinder the expansion thiophene of oxygen to matrix, and coating has good antioxidant property.
Test six: by test five ZrB that obtain 2-SiC/SiC ceramic coating carries out anti-oxidant test: by test five ZrB that obtain 2it is in the retort furnace of 1500 ℃ that-SiC/SiC ceramic coating is put into temperature, after insulation 30min, takes out, and at room temperature after cooling 30min, weighs, and repeats above-mentioned steps 15 times.
The test data curve that Figure 10 obtains for test six, curve 1 is figure of merit curve, and curve 2 is rate of weight loss curve, and as can be seen from the figure, sample is at the weightless 0.133g of sample after 15 loop tests, and rate of weight loss is 10.8%.This is the destruction that has caused coating due to the thermal stresses constantly producing due to sample in the high low temperature test process of circulation, produces oxygen and enters the passage of matrix, causes the continuous oxidation of matrix to cause.Can find out that from whole oxidation weight loss change curve this coating has good antioxidant property whole test process, and the high Low Temperature Thermal that coating can be born certain number of times impacts and does not destroy, after 15 high cold cycle, sample rate of weight loss is less than 11%, illustrate that the coating obtaining in test five has good antioxidant property, can effectively improve the oxidation-resistance of body material.
Test seven: a kind of ZrB of this test 2the preparation method of-SiC/SiC ceramic coating carries out according to the following steps:
One, the preparation of middle layer SiC: Si powder and Graphite Powder 99 are evenly mixed, obtain raw material 1; Raw material 1 is dry in rotatory evaporator after wet mixing ball milling mixes, obtain powder mix 1; With sand paper by base member to be coated polishing chamfering, adopt entrapping method that the base member to be coated of having polished is embedded in powder mix 1, obtain the base member of embedding powder mix 1, then under the condition that is 80Pa in vacuum tightness, the base member of embedding powder mix 1 being heated to temperature is 1800 ℃, and be to be incubated 2h under the condition of 1800 ℃ in temperature, cool to room temperature with the furnace, then, after ultrasonic cleaning and being dried, obtain the base member of embedding middle layer SiC; In raw material 1 described in step 1, the massfraction of Si powder is 82%, and the massfraction of Graphite Powder 99 is 18%;
Two, ZrB 2the preparation of-SiC/SiC ceramic coating: by ZrB 2powder, Si powder and Graphite Powder 99 evenly mix, and obtain raw material 3; Using ferrocene as additive 2; Additive 2 is dry in rotatory evaporator after wet mixing ball milling mixes with raw material 3, obtain powder mix 2; The base member of the embedding middle layer SiC that employing entrapping method obtains step 1 is embedded in powder mix 2, obtain the base member of embedding powder mix 2, then under the condition that is 80Pa in vacuum tightness, the base member of embedding powder mix 2 being heated to temperature is 2000 ℃, and be to be incubated 2h under the condition of 2000 ℃ in temperature, cool to room temperature with the furnace, obtain ZrB 2-SiC/SiC ceramic coating; ZrB in raw material 3 described in step 2 2the massfraction of powder is 73.7%, the massfraction of Si powder is 21%, the massfraction of Graphite Powder 99 is 5.3%; The massfraction of the additive 2 in the powder mix 2 described in step 2 is 5%; The batch mixing medium of the wet mixing ball milling described in step 1 and step 2 is alcohol; Base member to be coated described in step 1 is graphite.
Figure 11 is test seven ZrB that obtain 2the scanning electron photomicrograph of-SiC outer coating, can find out ZrB by this photo 2-SiC outer coating has more loose, and coatingsurface has space to exist, and this explanation coating can not effectively hinder the diffusion of oxygen to matrix, and the antioxidant property of coating is not as test five.
Test eight: by test seven ZrB that obtain 2-SiC/SiC ceramic coating carries out anti-oxidant test: by test seven ZrB that obtain 2it is in the retort furnace of 1500 ℃ that-SiC/SiC ceramic coating is put into temperature, after insulation 30min, takes out, and at room temperature after cooling 30min, weighs, and repeats above-mentioned steps 15 times.
The test data curve that Figure 12 obtains for test six, curve 1 is figure of merit curve, curve 2 is rate of weight loss curve, as can be seen from the figure, sample is at the weightless 0.3476g of sample after 15 loop tests, rate of weight loss is 31%, this is because sample is fine and close not and destroy to produce oxygen at the high low temperature test process floating coat of circulation and enter the passage of matrix and jointly cause the continuous oxidation of matrix to cause in coating itself, in the past the experiment situation of 5 times shows, through 4 circulation experiments, sample is weightless 0.062g only, and rate of weight loss is only 3%.This illustrates that this coating does not have certain antioxidant property in destruction situation, and the high Low Temperature Thermal that coating can be born certain number of times impacts and do not destroy, thus the ZrB that explanation test seven obtains 2-SiC/SiC ceramic coating has certain antioxidant property.

Claims (8)

1. a ZrB 2the preparation method of-SiC/SiC ceramic coating, is characterized in that ZrB 2the preparation method of-SiC/SiC ceramic coating carries out according to the following steps:
One, the preparation of middle layer SiC: Si powder and C powder are evenly mixed, obtain raw material 1; Si powder, C powder and SiC powder are evenly mixed, obtain raw material 2; By B 2o 3, Al 2o 3, a kind of in ferrocene and nickelocene or several mixture wherein, obtain additive 1; Additive 1 is dry in rotatory evaporator after wet mixing ball milling mixes with raw material 1 or raw material 2, obtain powder mix 1; With sand paper by base member to be coated polishing chamfering, adopt entrapping method that the base member to be coated of having polished is embedded in powder mix 1, obtain the base member of embedding powder mix 1, then the base member of embedding powder mix 1 being heated to temperature under vacuum or protective atmosphere is 1400 ℃～2200 ℃, and be to be incubated 10min～4h under the condition of 1400 ℃～2200 ℃ in temperature, cool to room temperature with the furnace, then, after ultrasonic cleaning and being dried, obtain the base member of embedding middle layer SiC; The massfraction of the additive 1 in the powder mix 1 described in step 1 is 0～18%; In raw material 1 described in step 1, the massfraction of Si powder is that the massfraction of 30%～85%, C powder is 15%～70%; The massfraction that in raw material 2 described in step 1, the massfraction of Si powder is 20%～80%, the massfraction of C powder is 2%～20%, SiC powder is that the massfraction summation of 3%～60%, Si powder, C powder and SiC powder is 100%;
Two, ZrB 2the preparation of-SiC/SiC ceramic coating: by ZrB 2powder, Si powder and C powder evenly mix, and obtain raw material 3; B powder, Zr powder and SiC powder are evenly mixed, obtain raw material 4; By ZrB 2powder, Si powder, C powder and SiC powder evenly mix, and obtain raw material 5; By B powder, Zr powder, SiC powder and ZrB 2powder evenly mixes, and obtains raw material 6; By ZrB 2powder, Si powder, C powder, SiC powder and B powder evenly mix, and obtain raw material 7; By ZrB 2powder, Si powder, C powder, SiC powder and Zr powder evenly mix, and obtain raw material 8; By B powder, Zr powder, SiC powder, ZrB 2powder and Si powder evenly mix, and obtain raw material 9; By ZrB 2powder, B powder, Zr powder, Si powder, C powder and SiC powder evenly mix, and obtain raw material 10; By SiO 2, B 2o 3, Al 2o 3, a kind of in ferrocene and nickelocene or several mixture wherein, obtain additive 2; Additive 2 is dry in rotatory evaporator after wet mixing ball milling mixes with raw material 3, raw material 4, raw material 5, raw material 6, raw material 7, raw material 8, raw material 9 or raw material 10, obtain powder mix 2; The base member of the embedding middle layer SiC that employing entrapping method obtains step 1 is embedded in powder mix 2; obtain the base member of embedding powder mix 2; then the base member of embedding powder mix 2 being heated to temperature under vacuum or protective atmosphere is 1400 ℃～3600 ℃; and be to be incubated 10min～6h under the condition of 1400 ℃～3600 ℃ in temperature; cool to room temperature with the furnace, obtain ZrB 2-SiC/SiC ceramic coating; The massfraction of the additive 2 in the powder mix 2 described in step 2 is 0～18%; ZrB in raw material 3 described in step 2 2the massfraction of powder is 50%～80%, the massfraction of Si powder is 3%～80%, the massfraction of C powder is 2%～20%, ZrB 2the massfraction summation of powder, Si powder and C powder is 100%; The massfraction summation that in raw material 4 described in step 2, the massfraction of B powder is 20%～50%, the massfraction of Zr powder is 10%～50%, the massfraction of SiC powder is 3%～50%, B powder, Zr powder and SiC powder is 100%; ZrB in raw material 5 described in step 2 2the massfraction of powder is 50%～80%, the massfraction of Si powder is 3%～80%, the massfraction of C powder is 2%～20%, the massfraction of SiC powder is 3%～50%, ZrB 2the massfraction summation of powder, Si powder, C powder and SiC powder is 100%; In raw material 6 described in step 2, B powder massfraction is 20%～50%, Zr powder massfraction is 10%～50%, SiC powder massfraction is 3%～50%, ZrB 2powder massfraction is 50%～80%, B powder, Zr powder, SiC powder and ZrB 2the massfraction summation of powder is 100%; ZrB in raw material 7 described in step 2 2powder massfraction is 50%～80%, Si powder massfraction is 3%～80%, C powder massfraction is 2%～20%, SiC powder massfraction is 3%～50%, B powder massfraction is 20%～50%, ZrB 2the massfraction summation of powder, Si powder, C powder, SiC powder and B powder is 100%; ZrB in raw material 8 described in step 2 2powder massfraction is 50%～80%, Si powder massfraction is 3%～80%, C powder massfraction is 2%～20%, SiC powder massfraction is 3%～50%, Zr powder massfraction is 10%～50%, ZrB 2the massfraction summation of powder, Si powder, C powder, SiC powder and Zr powder is 100%; In raw material 9 described in step 2, B powder massfraction is 20%～50%, Zr powder massfraction is 10%～50%, SiC powder massfraction is 3%～50%, ZrB 2powder massfraction is 50%～80%, Si powder massfraction is 3%～80%, B powder, Zr powder, SiC powder, ZrB 2the massfraction summation of powder and Si powder is 100%; ZrB in raw material 10 described in step 2 2powder massfraction is 50%～80%, B powder massfraction is 20%～50%, Zr powder massfraction is 10%～50%, Si powder massfraction is 3%～80%, C powder massfraction is 2%～20%, SiC powder massfraction is 3%～50%, ZrB 2the massfraction summation of powder, B powder, Zr powder, Si powder, C powder and SiC powder is 100%.
2. a kind of ZrB according to claim 1 2the preparation method of-SiC/SiC ceramic coating, is characterized in that the protection gas described in step 1 is argon gas or nitrogen, and the vacuum tightness described in step 1 is below 100Pa.
3. a kind of ZrB according to claim 1 2the preparation method of-SiC/SiC ceramic coating; it is characterized in that in step 1, the base member of embedding powder mix being heated to temperature under protective atmosphere is 1600 ℃～2000 ℃; and be to be incubated 1h～2h under the condition of 1600 ℃～2000 ℃ in temperature, cool to room temperature with the furnace.
4. a kind of ZrB according to claim 1 2the preparation method of-SiC/SiC ceramic coating, is characterized in that the batch mixing medium of the wet mixing ball milling described in step 1 and step 2 is alcohol.
5. a kind of ZrB according to claim 1 2the preparation method of-SiC/SiC ceramic coating, is characterized in that all C powder described in step 1 and step 2 are graphite or carbon black.
6. a kind of ZrB according to claim 1 2the preparation method of-SiC/SiC ceramic coating, is characterized in that the protection gas described in step 2 is argon gas or nitrogen, and the vacuum tightness described in step 2 is below 100Pa.
7. a kind of ZrB according to claim 1 2the preparation method of-SiC/SiC ceramic coating, is characterized in that the base member to be coated described in step 1 is graphite, C/C matrix material or C/SiC matrix material.
8. a kind of ZrB according to claim 1 2the preparation method of-SiC/SiC ceramic coating; it is characterized in that in step 2, the base member of embedding powder mix 2 being heated to temperature under protective atmosphere is 2000 ℃～3000 ℃; and be to be incubated 2h～4h under the condition of 2000 ℃～3000 ℃ in temperature, cool to room temperature with the furnace, obtain ZrB 2-SiC/SiC ceramic coating.
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