CN105237034A - Method for preparing porous silicon carbide ceramic based on template - Google Patents
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- CN105237034A CN105237034A CN201510577885.6A CN201510577885A CN105237034A CN 105237034 A CN105237034 A CN 105237034A CN 201510577885 A CN201510577885 A CN 201510577885A CN 105237034 A CN105237034 A CN 105237034A
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Abstract
The present invention relates to a method for preparing a porous silicon carbide ceramic based on a template. According to the present invention, the template method thinking and the characteristics of the CVI process are creatively combined, the CVI method is used to prepare the porous SiC ceramic, and the porous SiC ceramic obtained through the method has characteristics of uniform pore size, controlled porosity and large specific surface area; with the method, the technical problems of complex preparation process, high sintering temperature and the like of other template methods can be solved; and the complex member is easily prepared through the process, and the use range of the porous SiC ceramic prepared through the method is substantially expanded.
Description
Technical field
The invention belongs to porous silicon carbide ceramic preparation method, be specifically related to a kind of method adopting Template preparation porous silicon carbide ceramic.
Background technology
Porous silicon carbide ceramic is that a kind of inside has and communicates in a large number or the new ceramic material of closed pore passage structure, because it has low density, high strength, specific surface area is large, performances such as excellent thermostability and chemical stability and be widely applied in industry, as hot gas particulate strainer, filter for molten metal, support of the catalyst, gaseous combustion medium, lightweight structural parts etc.
The method preparing porous SiC ceramics has a lot, as sintering process, and foaming, mull technique, template etc.In order to regulate and control the porosity of porous SiC ceramics better, pore size distribution and pore appearance, template becomes the study hotspot of people gradually.Template refers to by hybrid template and SiC particle or SiC organic precursor, forms a kind of matrix material of two-phase mixtures, then removes template and sinters and obtain porous SiC ceramics.Be raw material with SiC powder in document " S.H.LeeandY.W.Kim; ProcessingofCellularSiCCeramicsUsingPolymerMicrobeads [J] .J.KoreanCeram.Soc.; 43; 458 – 462 (2006). ", take Al2O3-Y2O3 as sintering aid, take polymer microballoon as formwork frame, first three kinds of materials are mixed and be pressed into definite shape, this mixture burns of thermal treatment removing polymer microballoon again, form the biscuit with certain pore texture, last sintered body obtains required porous SiC ceramics material.By controlling the content of polymer microballoon and the temperature of sintering, the void content of porous SiC ceramics can be controlled between 16% ~ 69%.The porous SiC ceramics porous nickel that this legal system is standby, and when porosity is 40%, intensity can reach 40MPa, and intensity is higher, but this method sintering temperature is higher, and temperature, higher than 1700 DEG C, is unfavorable for that cost reduces.In document " Y.J.JinandY.W.Kim; Lowtemperatureprocessingofhighlyporoussiliconcarbidecera micswithimprovedflexuralstrength [J] .J.Mater.Sci.; 45; 282 – 285 (2010). ", using Polycarbosilane as SiC precursor, take polymer microballoon as formwork frame, take polysiloxane as binding agent, dry at 200 DEG C after mixing, then under 1100 ~ 1400 DEG C of conditions, carry out thermolysis, finally obtain porous SiC ceramics.The scope of the porous ceramics hole rate that this method obtains, between 60% ~ 90%, be also can reach 30MPa, but still there is the higher problem of sintering temperature in this method when void content is 70%.In document " M.Fukushima; M.Nakata; Y.Zhou; T.OhjiandY.Yoshizawa, Fabricationandpropertiesofultrahighlyporoussiliconcarbid ebythegelation – freezingmethod [J] .J.Eur.Ceram.Soc., 30; 2889 – 2896 (2010). ", with gel, water and SiC particle are raw material, adopt the standby porous SiC ceramics going out to have the high porosity aligned of gel refrigeration drying legal system.This method can prepare the parts of different shape, and the pore diameter of porous ceramics can be controlled within the scope of 34 ~ 147 μm by changing freezing temp, but this method also exists complex process, the problem that sintering temperature is higher.
Chemical vapour deposition (ChemicalVaporDeposition is called for short CVD) technology is grown up by the needs of Surface Engineering at first.Afterwards, people's guiding gas was deep into porous material inside deposition to reach the object making densifying materials, and then developed chemical vapor infiltration technology (ChemicalVaporInfiltration is called for short CVI).Material internal densification is that the generation of ceramic phase causes, this kind of ceramic phase can play filling and cohesive action, and, SiC ceramic can be made to be rendered as the form of nano wire mutually by catalyzer, greatly can promote the specific surface area of porous ceramics, for preparation, there is larger reference area and the controlled porous SiC ceramics of hole provides possibility.It is low that CVI method has preparation temperature, is easy to prepare the advantages such as complex component, more and more receives the concern of people.
Summary of the invention
The technical problem solved
More complicated in order to solve the preparation technology existed in porous silicon carbide ceramic prior art, sintering temperature is higher, etc. technical problem, the present invention proposes a kind of employing template, SiC ceramic phase is deposited again in template, form porous silicon carbide ceramic, finally again in porous ceramics growth inside SiC nanowire, and then obtain the method for the porous SiC ceramics had compared with bigger serface.
Technical scheme
Based on a method for Template preparation porous silicon carbide ceramic, it is characterized in that step is as follows:
Step 1: the template of processing according to design requirements is put into chemical vapor infiltration poke CVI stove, with MTSCH
3siCl
3as precursor, hydrogen is as carrier gas and diluent gas, and argon gas carries out chemical vapor infiltration as shielding gas; In CVI process, the SiC ceramic of generation covers mutually in template and obtains porous SiC ceramics; Described template is nickel foam, foamy carbon or metal foam template;
Step 2, remove template: when template be nickel foam or metal foam template time adopt souring method remove template, the method utilizing low-temperature oxidation burn when template is foamy carbon removal template, obtain porous SiC ceramics.
After step 2 completes, the porous SiC ceramics obtained is put into again chemical vapor infiltration poke CVI stove, with MTSCH
3siCl
3as precursor, hydrogen is as carrier gas and diluent gas, and argon gas, as shielding gas deposition preparation SiC nanowire, to regulate porous ceramics hole, improves the specific surface area of porous ceramics.
The porosity ranges of described template is 40% ~ 90%.
In described step 1 in CVI process MTS: H
2: the ratio of Ar is 1: 5 ~ 15: 10 ~ 20.
In described step 1, in CVI process, processing parameter is: total gas pressure is 0.5 ~ 5kPa, and depositing temperature is 900-1200 DEG C, and depositing time is 10 ~ 200h.
In described step 2, the combustion reference temperature of low-temperature oxidation burning is 400 ~ 700 DEG C.
Any one or the multiple combination that add the muriate of Fe, Co, Ni or nitrate during described preparation SiC nanowire are catalyzer.
The processing parameter of described preparation SiC nanowire is total gas pressure is 0.5 ~ 5kPa, and depositing temperature is 800-1100 DEG C, and depositing time is 1 ~ 10h.
During described preparation SiC nanowire MTS: H
2: the ratio of Ar is 1: 5 ~ 20: 3 ~ 15.
Beneficial effect
A kind of method based on Template preparation porous silicon carbide ceramic that the present invention proposes, creatively the feature of the thought of template with CVI technique is combined, propose to adopt CVI legal system for porous SiC ceramics, the porous SiC ceramics aperture that this method obtains is comparatively even, and controlled porosity, material has very large specific surface area.The preparation technology that the method can solve the appearance of other template is more complicated, and sintering temperature is high-technology problem comparatively, and this technique is easy to prepare complex component, greatly extends the use range of the standby porous SiC ceramics of this legal system.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of this technique
Fig. 2 is the pattern of the porous ceramics taking nickel foam as Template preparation
Fig. 3 is the enlarged view of porous ceramic surface SiC nanowire
Embodiment
Embodiment one
Step 1: raw material prepares: template adopts nickel foam, and void content is 40%.
Step 2: template is processed into designated shape.
Step 3: the difform template obtained in step 2 is put into chemical vapor infiltration poke (CVI stove) and carry out chemical vapor infiltration, in CVI process, the SiC ceramic generated covers in template mutually gradually, just can be formed when the SiC ceramic generated acquires a certain degree mutually and there is some strength, the porous SiC ceramics of controlled porosity.The processing condition that CVI method generates SiC ceramic phase are: utilize MTS (CH
3siCl
3) as precursor, hydrogen is as carrier gas and diluent gas, and argon gas is as shielding gas.MTS:H
2: the ratio of Ar is 1:12:10, and total gas pressure is 5kPa, and depositing temperature is 1000 DEG C, and depositing time is 20h.
Step 4: remove template.By the porous SiC ceramics acidification obtained.
Step 5: deposition SiC nanowire.The porous ceramics inside deposition obtained in step 4 prepares SiC nanowire, regulates porous ceramics hole further, improves the specific surface area of porous ceramics.The depositing operation of SiC nanowire is: utilize MTS (CH
3siCl
3) as precursor, hydrogen is as carrier gas and diluent gas, and argon gas is as shielding gas.MTS:H
2: the ratio of Ar is 1:5 ~ 20:3 ~ 15, and total gas pressure is 0.5 ~ 5kPa, and depositing temperature is 800-1100 DEG C, and depositing time is 1 ~ 10h.Any one or multiple combination of the catalyzer the used muriate that is Fe, Co, Ni or nitrate.Finally, can obtain that there is comparatively bigger serface, and the porous SiC ceramics that hole is controlled.
Embodiment two
Step 1: raw material prepares: template adopts nickel foam, and void content is 60%.
Step 2: template is processed into designated shape.
Step 3: the difform template obtained in step 2 is put into chemical vapor infiltration poke (CVI stove) and carry out chemical vapor infiltration, in CVI process, the SiC ceramic generated covers in template mutually gradually, just can be formed when the SiC ceramic generated acquires a certain degree mutually and there is some strength, the porous SiC ceramics of controlled porosity.The processing condition that CVI method generates SiC ceramic phase are: utilize MTS (CH
3siCl
3) as precursor, hydrogen is as carrier gas and diluent gas, and argon gas is as shielding gas.MTS:H
2: the ratio of Ar is 1:12:10, and total gas pressure is 5kPa, and depositing temperature is 1000 DEG C, and depositing time is 50h.
Step 4: remove template.By the porous SiC ceramics acidification obtained.
Step 5: deposition SiC nanowire.The porous ceramics inside deposition obtained in step 4 prepares SiC nanowire, regulates porous ceramics hole further, improves the specific surface area of porous ceramics.The depositing operation of SiC nanowire is: utilize MTS (CH
3siCl
3) as precursor, hydrogen is as carrier gas and diluent gas, and argon gas is as shielding gas.MTS:H
2: the ratio of Ar is 1:5 ~ 20:3 ~ 15, and total gas pressure is 0.5 ~ 5kPa, and depositing temperature is 800-1100 DEG C, and depositing time is 1 ~ 10h.Any one or multiple combination of the catalyzer the used muriate that is Fe, Co, Ni or nitrate.Finally, can obtain that there is comparatively bigger serface, and the porous SiC ceramics that hole is controlled.
Embodiment three
Step 1: raw material prepares: template adopts nickel foam, and void content is 70%.
Step 2: template is processed into designated shape.
Step 3: the difform template obtained in step 2 is put into chemical vapor infiltration poke (CVI stove) and carry out chemical vapor infiltration, in CVI process, the SiC ceramic generated covers in template mutually gradually, just can be formed when the SiC ceramic generated acquires a certain degree mutually and there is some strength, the porous SiC ceramics of controlled porosity.The processing condition that CVI method generates SiC ceramic phase are: utilize MTS (CH
3siCl
3) as precursor, hydrogen is as carrier gas and diluent gas, and argon gas is as shielding gas.MTS:H
2: the ratio of Ar is 1:12:10, and total gas pressure is 5kPa, and depositing temperature is 1100 DEG C, and depositing time is 20h.
Step 4: remove template.By the porous SiC ceramics acidification obtained.
Step 5: deposition SiC nanowire.The porous ceramics inside deposition obtained in step 4 prepares SiC nanowire, regulates porous ceramics hole further, improves the specific surface area of porous ceramics.The depositing operation of SiC nanowire is: utilize MTS (CH
3siCl
3) as precursor, hydrogen is as carrier gas and diluent gas, and argon gas is as shielding gas.MTS:H
2: the ratio of Ar is 1:5 ~ 20:3 ~ 15, and total gas pressure is 0.5 ~ 5kPa, and depositing temperature is 800-1100 DEG C, and depositing time is 1 ~ 10h.Any one or multiple combination of the catalyzer the used muriate that is Fe, Co, Ni or nitrate.Finally, can obtain that there is comparatively bigger serface, and the porous SiC ceramics that hole is controlled.
Embodiment four
Step 1: raw material prepares: template adopts nickel foam, and void content is 90%.
Step 2: template is processed into designated shape.
Step 3: the difform template obtained in step 2 is put into chemical vapor infiltration poke (CVI stove) and carry out chemical vapor infiltration, in CVI process, the SiC ceramic generated covers in template mutually gradually, just can be formed when the SiC ceramic generated acquires a certain degree mutually and there is some strength, the porous SiC ceramics of controlled porosity.The processing condition that CVI method generates SiC ceramic phase are: utilize MTS (CH
3siCl
3) as precursor, hydrogen is as carrier gas and diluent gas, and argon gas is as shielding gas.MTS:H
2: the ratio of Ar is 1:12:10, and total gas pressure is 5kPa, and depositing temperature is 1100 DEG C, and depositing time is 50h.
Step 4: remove template.By the porous SiC ceramics acidification obtained.
Step 5: deposition SiC nanowire.The porous ceramics inside deposition obtained in step 4 prepares SiC nanowire, regulates porous ceramics hole further, improves the specific surface area of porous ceramics.The depositing operation of SiC nanowire is: utilize MTS (CH
3siCl
3) as precursor, hydrogen is as carrier gas and diluent gas, and argon gas is as shielding gas.MTS:H
2: the ratio of Ar is 1:5 ~ 20:3 ~ 15, and total gas pressure is 0.5 ~ 5kPa, and depositing temperature is 800-1100 DEG C, and depositing time is 1 ~ 10h.Any one or multiple combination of the catalyzer the used muriate that is Fe, Co, Ni or nitrate.Finally, can obtain that there is comparatively bigger serface, and the porous SiC ceramics that hole is controlled.
Embodiment five
Step 1: raw material prepares: template adopts foamy carbon, and void content is 70%.
Step 2: template is processed into designated shape.
Step 3: the difform template obtained in step 2 is put into chemical vapor infiltration poke (CVI stove) and carry out chemical vapor infiltration, in CVI process, the SiC ceramic generated covers in template mutually gradually, just can be formed when the SiC ceramic generated acquires a certain degree mutually and there is some strength, the porous SiC ceramics of controlled porosity.The processing condition that CVI method generates SiC ceramic phase are: utilize MTS (CH
3siCl
3) as precursor, hydrogen is as carrier gas and diluent gas, and argon gas is as shielding gas.MTS:H
2: the ratio of Ar is 1:12:10, and total gas pressure is 5kPa, and depositing temperature is 1000 DEG C, and depositing time is 20h.
Step 4: remove template.By the porous SiC ceramics 500 DEG C of oxidation removal foamy carbon templates obtained.
Step 5: deposition SiC nanowire.The porous ceramics inside deposition obtained in step 4 prepares SiC nanowire, regulates porous ceramics hole further, improves the specific surface area of porous ceramics.The depositing operation of SiC nanowire is: utilize MTS (CH
3siCl
3) as precursor, hydrogen is as carrier gas and diluent gas, and argon gas is as shielding gas.MTS:H
2: the ratio of Ar is 1:5 ~ 20:3 ~ 15, and total gas pressure is 0.5 ~ 5kPa, and depositing temperature is 800-1100 DEG C, and depositing time is 1 ~ 10h.Any one or multiple combination of the catalyzer the used muriate that is Fe, Co, Ni or nitrate.Finally, can obtain that there is comparatively bigger serface, and the porous SiC ceramics that hole is controlled.
Embodiment six
Step 1: raw material prepares: template adopts foamy carbon, and void content is 90%.
Step 2: template is processed into designated shape.
Step 3: the difform template obtained in step 2 is put into chemical vapor infiltration poke (CVI stove) and carry out chemical vapor infiltration, in CVI process, the SiC ceramic generated covers in template mutually gradually, just can be formed when the SiC ceramic generated acquires a certain degree mutually and there is some strength, the porous SiC ceramics of controlled porosity.The processing condition that CVI method generates SiC ceramic phase are: utilize MTS (CH
3siCl
3) as precursor, hydrogen is as carrier gas and diluent gas, and argon gas is as shielding gas.MTS:H
2: the ratio of Ar is 1:12:10, and total gas pressure is 5kPa, and depositing temperature is 1100 DEG C, and depositing time is 20h.
Step 4: remove template.By the porous SiC ceramics 500 DEG C of oxidation removal foamy carbon templates obtained.
Step 5: deposition SiC nanowire.The porous ceramics inside deposition obtained in step 4 prepares SiC nanowire, regulates porous ceramics hole further, improves the specific surface area of porous ceramics.The depositing operation of SiC nanowire is: utilize MTS (CH
3siCl
3) as precursor, hydrogen is as carrier gas and diluent gas, and argon gas is as shielding gas.MTS:H
2: the ratio of Ar is 1:5 ~ 20:3 ~ 15, and total gas pressure is 0.5 ~ 5kPa, and depositing temperature is 800-1100 DEG C, and depositing time is 1 ~ 10h.Any one or multiple combination of the catalyzer the used muriate that is Fe, Co, Ni or nitrate.Finally, can obtain that there is comparatively bigger serface, and the porous SiC ceramics that hole is controlled.
Claims (9)
1., based on a method for Template preparation porous silicon carbide ceramic, it is characterized in that step is as follows:
Step 1: the template of processing according to design requirements is put into chemical vapor infiltration poke CVI stove, with MTSCH
3siCl
3as precursor, hydrogen is as carrier gas and diluent gas, and argon gas carries out chemical vapor infiltration as shielding gas; In CVI process, the SiC ceramic of generation covers mutually in template and obtains porous SiC ceramics; Described template is nickel foam, foamy carbon or metal foam template;
Step 2, remove template: when template be nickel foam or metal foam template time adopt souring method remove template, the method utilizing low-temperature oxidation burn when template is foamy carbon removal template, obtain porous SiC ceramics.
2. according to claim 1 based on the method for Template preparation porous silicon carbide ceramic, it is characterized in that: after step 2 completes, the porous SiC ceramics obtained is put into chemical vapor infiltration poke CVI stove, with MTSCH again
3siCl
3as precursor, hydrogen is as carrier gas and diluent gas, and argon gas, as shielding gas deposition preparation SiC nanowire, to regulate porous ceramics hole, improves the specific surface area of porous ceramics.
3. according to claim 1 based on the method for Template preparation porous silicon carbide ceramic, it is characterized in that: the porosity ranges of described template is 40% ~ 90%.
4. according to claim 1 based on the method for Template preparation porous silicon carbide ceramic, it is characterized in that: in described step 1 in CVI process MTS: H
2: the ratio of Ar is 1: 5 ~ 15: 10 ~ 20.
5. according to claim 1 based on the method for Template preparation porous silicon carbide ceramic, it is characterized in that: in described step 1, in CVI process, processing parameter is: total gas pressure is 0.5 ~ 5kPa, depositing temperature is 900-1200 DEG C, and depositing time is 10 ~ 200h.
6. according to claim 1 based on the method for Template preparation porous silicon carbide ceramic, it is characterized in that: in described step 2, the combustion reference temperature of low-temperature oxidation burning is 400 ~ 700 DEG C.
7. according to claim 2 based on the method for Template preparation porous silicon carbide ceramic, it is characterized in that: any one or the multiple combination that add the muriate of Fe, Co, Ni or nitrate during described preparation SiC nanowire are catalyzer.
8. according to claim 2 or 7 based on the method for Template preparation porous silicon carbide ceramic, it is characterized in that: the processing parameter of described preparation SiC nanowire is total gas pressure is 0.5 ~ 5kPa, and depositing temperature is 800-1100 DEG C, and depositing time is 1 ~ 10h.
9. according to claim 2 or 7 based on the method for Template preparation porous silicon carbide ceramic, it is characterized in that: during described preparation SiC nanowire MTS: H
2: the ratio of Ar is 1: 5 ~ 20: 3 ~ 15.
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| CN111807842A (en) * | 2020-07-07 | 2020-10-23 | 山东大学 | Porous silicon carbide ceramic material and preparation method thereof |
| CN111925229A (en) * | 2020-07-12 | 2020-11-13 | 西北工业大学 | Method for preparing high-performance foamed ceramic by combining template method with chemical vapor infiltration method |
| CN113658724A (en) * | 2021-08-17 | 2021-11-16 | 西北工业大学 | Ceramic composite fuel pellet and preparation method and application thereof |
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