CN103992127A - Method for preparing carbon/carbon composite material and lithium aluminosilicate glass ceramic joint - Google Patents
Method for preparing carbon/carbon composite material and lithium aluminosilicate glass ceramic joint Download PDFInfo
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- CN103992127A CN103992127A CN201410232658.5A CN201410232658A CN103992127A CN 103992127 A CN103992127 A CN 103992127A CN 201410232658 A CN201410232658 A CN 201410232658A CN 103992127 A CN103992127 A CN 103992127A
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Abstract
The invention relates to a method for preparing a carbon/carbon composite material and a lithium aluminosilicate glass ceramic joint. Silicon carbide (SiC) ceramic is taken as a transition layer, so that adverse high-temperature interfacial reaction between the C/C composite material and LAS (lithium aluminosilicate) glass ceramic can be blocked and the problem of poor wettability of LAS glass ceramic on the surface of the C/C composite material can be improved; low-expansion ZnO-Al2O3-SiO2 (ZAS) glass is taken as an intermediate connection layer, so that the thermal mismatch between SiC and LAS can be relieved and connection is performed through a vacuum hot pressing technology. By regulating a hot-pressing temperature program, glass of the intermediate layer becomes a main crystal phase which is ZAS glass ceramic of sanidine and zinc feldspar, the thermal expansion coefficient is close to the thermal expansion coefficient of C/C and LAS, the thermal stress at an interface is effectively relieved, the prepared C/C-ZAS-LAS joint has good performances and the shear strength of the joint achieves 24.59MPa-30.06MPa.
Description
Technical field
The present invention relates to one and prepare the method for carbon/carbon (C/C) matrix material and lithium aluminium silicon (LAS) glass-ceramic joint, a kind of ZnO-Al preparing with oneself
2o
3-SiO
2(ZAS) glass is intermediate connecting layer, and connects by vacuum hot-pressing process.By regulating hot pressing temperature program, make middle layer glass become the low thermal expansion glass pottery taking saturating zinc feldspar as principal crystalline phase, the thermal expansivity of its thermal expansivity and C/C and LAS is close, and has effectively alleviated the thermal stresses of interface, prepares well behaved C/C-LAS joint.
Background technology
LAS glass-ceramic has the high-temperature behavior of the excellences such as low bulk, high temperature resistant, anti-thermal shock and is applied to the fields such as high-temperature electric light source glass, high-temperature observation window and modern technical aeronautics.But due to the intrinsic fragility of LAS glass-ceramic self own, under plus load effect, very easily rupture.C/C matrix material has lightweight, a series of excellent properties such as modulus is high, thermal expansivity is low, heat shock resistance are a kind of novel fire resistant structured materials.Thereby LAS glass-ceramic and C/C matrix material are coupled together and can merge the two structure and functionality advantage, improve the supporting capacity of web member entirety, reduce the density of member, be applied to aerospace field thereby can be used as high temperature functional structure matrix material.But C/C matrix material and LAS glass-ceramic are foreign materials, exist obvious physicochemical property difference between the two, while directly connection, gained joint performance is not high.If adopt reliable and stable vacuum hotpressing interconnection technique, taking silicon carbide ceramics (SiC) as transition layer, the bad high-temperature interface that can intercept between C/C and LAS glass-ceramic reacts and improves LAS glass-ceramic in the poor problem of C/C composite material surface wettability; And with the principal crystalline phase of low bulk be the ZnO-Al of zinc feldspar
2o
3-SiO
2(ZAS) devitrified glass is intermediate connecting layer, alleviates the thermal mismatching between SiC-LAS.And then obtain well behaved C/C-LAS joint.
Document 1 " both at home and abroad carbon/carbon compound material connects progress [J]. Lan Fengtao; Li Kezhi; Li Hejun; etc. material Leader; 23 (2009) 9 – 12. " connect C/C and LAS taking SiC as transition layer, although effectively improved the problem that LAS reacts at the nonwetting and bad high-temperature interface in C/C surface.But the thermal expansion mismatch problem between SiC-LAS is not still resolved.
Document 2 " C/C matrix material is connected with LAS glass-ceramic. Lin Xiaoqiu. and the master thesis .2008. of Northwestern Polytechnical University " with MgO-Al
2o
3-SiO
2-B
2o
3, MgO-Al
2o
3-SiO2-TiO
2, Y
2o
3-Al
2o
3-SiO
2-TiO
2connect C/C and LAS etc. different glass intermediate connecting layers, wherein adopt Y
2o
3-Al
2o
3-SiO
2-TiO
2glass-ceramic is as middle layer best results, and the high shear strength of gained can also only have the 26.21MPa of reaching, and used but due to Y
2o
3expensive raw material price, owing to being subject to the restriction of mechanical strength of these several articulamentums itself, prepared C/C-LAS joint is still lower than 27MPa in addition.
Document 3 " CeO
2the impact of modification MAS middle layer on C/C-LAS jointing performance. Zhu Huanxia. the master thesis .2013. of Northwestern Polytechnical University " although by adding Rare-Earth Ce O
2modification MAS middle layer, but owing to being subject to the restriction of the mechanical property in MAS middle layer own, even in the time that optimum addition is 0.5wt.%, the average shear intensity of joint is for being only 25.37MPa, and high shear strength is only 26.75MPa, and Rare-Earth Ce O used
2expensive.
Document 4 " ZnO-Al
2o
3-SiO
2the hot expansibility of microcrystalline glass in series and influence factor thereof [J]. Wang Minquan, Yu Zhichu, Cheng Feng. glass industry .1986,6 (2): 36 " and " Rahaman M.N.Ceramic processing and sintering[M] .Marcel.Dekker.New York.Inc.1995:102～104 " literary composition in the ZnO-Al that principal crystalline phase is zinc feldspar is proposed
2o
3-SiO
2(ZAS) devitrified glass not only has excellent mechanical property, and have and C/C matrix material and the very approaching low thermal coefficient of expansion of LAS glass-ceramic, the devitrified glass that some mechanical property such as its bending strength is prepared than LAS is more superior, and made flat board has been applied to industrial technology aspect.Therefore select the intermediate connecting layer of ZAS glass as C/C and LAS, can obtain reliable joint.
Summary of the invention
The technical problem solving
In order to solve the weak point of existing issue, the present invention proposes a kind of method of preparing carbon/carbon compound material and lithium aluminosilicate glass ceramic joint.Taking silicon carbide ceramics (SiC) as transition layer, the bad high-temperature interface that can intercept between C/C matrix material and LAS glass-ceramic reacts and improves LAS glass-ceramic in the poor problem of C/C composite material surface wettability; And with the principal crystalline phase of low bulk be the ZnO-Al of zinc feldspar
2o
3-SiO
2(ZAS) devitrified glass is intermediate connecting layer, alleviates the thermal mismatching between SiC-LAS.And then obtain well behaved C/C-LAS joint.
Technical scheme
A method of preparing carbon/carbon compound material and lithium aluminosilicate glass ceramic joint, is characterized in that step is as follows:
Step 1: the Si powder that is 60～80% by massfraction, 15～25% C powder and 5～15% Al
2o
3powder mixing and ball milling 1～3h post-drying obtains mixed powder; Mixed powder is packed in plumbago crucible, and carbon/carbon compound material C/C is embedded in mixed powder; Then plumbago crucible is placed in to vacuum high-temperature Reaktionsofen, using argon gas as shielding gas, with the heat-up rate of 5～10 DEG C/min by furnace temperature to 2000～2200 DEG C, insulation 1～3h, powered-down naturally cools to room temperature by it subsequently, obtains the C/C matrix material with SiC transition layer; Described carbon/carbon compound material C/C is ultrasonic cleaning oven dry in dehydrated alcohol;
Step 2: ZAS glass powder is made to serum taking dehydrated alcohol as dispersant, and brushing, on to be connected of the C/C matrix material with SiC transition layer, is placed in 80～100 DEG C of baking ovens and dries.
Step 3: the C/C matrix material that step 2 is dried is placed in the hot pressing die of high-strength graphite material, pours LAS glass powder into be connected and goes up and tile evenly, then grinding tool is put into vacuum hotpressing stove;
Step 4: first to hot pressing furnace extracting vacuum, below being extracted into negative pressure time, with 5～10 DEG C/min heat-up rate, furnace temperature is risen to 1200～1300 DEG C from room temperature, insulation 15～45min also loads 20～25MPa pressure, after finishing, insulation closes heating power supply with stove naturally cooling, release in the time that temperature drops to 1000 DEG C, the carbon/carbon compound material-lithium aluminosilicate glass ceramic joint obtaining that takes out while continuing to be cooled to room temperature to be cooled.
The preparation of described ZAS glass powder: the Li that is 10～18% by massfraction
2cO
3powder, 10～20% Al
2o
3powder and 55～75% SiO
2powder, puts into the oxidized still that corundum crucible is built in 1500～1600 DEG C and is incubated 3～5h after mixing and ball milling 1～3h, carry out at once shrend after taking-up, obtains LAS glass block; Then by LAS glass block crushing drying, taking distilled water as medium wet-milling 9～11h post-drying, cross 300 mesh sieves, finally obtain LAS glass powder.
The preparation of described ZAS glass powder: the ZnO powder that is 15～25% by massfraction, 10～20% Al
2o
3powder, 60～75% SiO
2powder, 2～5% TiO
2powder and 0.5% Sb
2o
3, ball milling mixes to be put into the oxidized still that corundum crucible is built in 1500～1600 DEG C after 1～3h and is incubated 3～5h, carries out at once shrend after taking-up, obtains ZAS glass block; Then by ZAS glass block crushing drying, taking distilled water as medium wet-milling 9～11h post-drying, cross 300 mesh sieves, finally obtain ZAS glass powder.
When preparation LAS glass powder, add micro-TiO
2, B
2o
3and Sb
2o
3powder.
Described C powder and Si powder purity are 99%, and granularity is 300 orders.
Described Li
2cO
3powder, Al
2o
3powder and SiO
2powder is analytical pure, and purity is not less than 97%, and granularity is 300 orders.
Described ZnO powder, Al
2o
3powder, SiO
2powder, TiO
2powder and Sb
2o
3be analytical pure, purity is not less than 97%, and granularity is 300 orders.
Described TiO
2, B
2o
3and Sb
2o
3powder is analytical pure, and purity is not less than 97%, and granularity is 300 orders.
The negative pressure state of described step 4 is furnace pressure ∠ 10
-1p
a.
A kind of method of preparing carbon/carbon compound material and lithium aluminosilicate glass ceramic joint that the present invention proposes, taking silicon carbide ceramics (SiC) as transition layer, the bad high-temperature interface that can intercept between C/C matrix material and LAS glass-ceramic reacts and improves LAS glass-ceramic in the poor problem of C/C composite material surface wettability; And with the ZnO-Al of low bulk
2o
3-SiO
2(ZAS) glass is intermediate connecting layer, alleviates the thermal mismatching between SiC-LAS, and connects by vacuum hot-pressing process.By regulating hot pressing temperature program, make middle layer glass become the ZAS glass-ceramic that principal crystalline phase is zinc feldspar, the thermal expansivity of its thermal expansivity and C/C and LAS is close, effectively alleviate the thermal stresses of interface, the C/C-ZAS-LAS joint performance of preparing is good, and the shearing resistance of joint reaches 24.59MPa～30.06MPa.
Beneficial effect is: be that transition layer connects C/C and LAS because adopting SiC, effectively alleviated the problem of glass in the difficult wetting and bad high-temperature interface reaction in C/C surface.The principal crystalline phase that adopts low bulk is the ZnO-Al of new feldspar
2o
3-SiO
2(ZAS) devitrified glass is intermediate connecting layer, alleviates the thermal mismatching between SiC-LAS, and then obtains the joint of well behaved C/C-LAS, and the shearing resistance of gained joint reaches 24.59MPa～30.06MPa.
Brief description of the drawings
Fig. 1 is the interface SEM picture of the prepared C/C-LAS joint of the embodiment of the present invention 3.
Fig. 2 is the shearing area SEM picture of the prepared C/C-LAS joint of the embodiment of the present invention 3 and the XRD figure of section spectrum.
Fig. 3 is the joint of the prepared C/C-LAS of the embodiment of the present invention 3 load-displacement curve figure in shearing test.
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Embodiment 1:
Step 1: processed 30mm × 30mm × 4mm C/C matrix material is put into dehydrated alcohol ultrasonic cleaning, be then placed in baking oven dry for standby at 100 DEG C.
Step 2: take respectively massfraction and be 70% Si powder, 20% C powder and 10% Al
2o
3powder, takes out these three kinds of powders with ball mill mixing and ball milling 2h, be then placed in baking oven 30min at 100 DEG C and dry; A dry blending powder part for preparation is first encased in to about 4cm thickness in plumbago crucible, after the C/C matrix material sanding and polishing that band is connected cleaning, drying, put on it, then another part being laid in to (its thickness is with being about equally 4cm) on C/C matrix material, even if C/C matrix material is embedded in mixed powder; Then plumbago crucible is placed in to vacuum high-temperature Reaktionsofen, using argon gas as shielding gas, with the heat-up rate of 10 DEG C/min by furnace temperature to 2000 DEG C, insulation 3h, powered-down naturally cools to room temperature by it subsequently, obtains the C/C matrix material sample with SiC transition layer;
Step 3: take respectively massfraction and be 15% Li
2cO
3powder, 13% Al
2o
3powder, 70% SiO
2powder, is incubated 5h by these powders with putting into the oxidized still that corundum crucible is built in 1500 DEG C after ball mill mixing and ball milling 2h, carries out at once shrend after taking-up, obtains LAS glass block; Then broken, oven dry then, after wet-milling (taking distilled water as medium) 11h, is dried 36h, is crossed 300 mesh sieves in 100 DEG C of baking ovens, finally obtains LAS glass powder for subsequent use;
When preparation LAS glass powder, add micro-TiO
2, B
2o
3and Sb
2o
3powder.
Step 4: taking respectively massfraction is 20% ZnO powder, 16% Al
2o
3powder, 60% SiO
2powder, 3%TiO
2powder and 0.5%Sb
2o
3, these powders are incubated to 5h with putting into the oxidized still that corundum crucible is built in 1550 DEG C after ball mill ball milling mixing 1h, after taking-up, carry out at once shrend, obtain ZAS glass block; Then oven dry, fragmentation then dried 36h after wet-milling (taking distilled water as medium) 11h in 100 DEG C of baking ovens, crosses 300 mesh sieves, finally obtains ZAS glass powder for subsequent use;
Step: 5: take the ZAS glass powder 1.5g and the 1.5ml dehydrated alcohol that are obtained by step 4, both are mixed and made into serum, then brush on the C/C matrix material specimen surface with SiC transition layer of being prepared by step 2 (being face to be connected), be then placed in 80 DEG C of baking ovens and dry 30min; After oven dry, be placed in the hot pressing die of high-strength graphite material, more prepared LAS glass powder 18g is poured on it and tiled evenly, then grinding tool is put into vacuum hotpressing stove;
Step 6: first to hot pressing furnace extracting vacuum, below being extracted into negative pressure time, with 5 DEG C/min heat-up rate, furnace temperature is risen to 1250 DEG C from room temperature again, insulation 15min also loads 20MPa pressure, after finishing, insulation closes heating power supply with stove naturally cooling, release in the time that temperature drops to 1000 DEG C, the sample that is processed into 12mm × 8mm × 6mm that takes out while continuing to be cooled to room temperature to be cooled does the shearing test under room temperature.Shearing test result shows, prepared joint average shear intensity is 24.59MPa.
Embodiment 2:
Step 1: the C/C matrix material of processed 30mm × 30mm × 4mm is put into dehydrated alcohol ultrasonic cleaning, be then placed in baking oven dry for standby at 100 DEG C.
Step 2: take respectively massfraction and be 65% Si powder, 25% C powder and 10% Al
2o
3powder, takes out these three kinds of powders with ball mill mixing and ball milling 2h, be then placed in baking oven 30min at 100 DEG C and dry; A dry blending powder part for preparation is first encased in to about 4cm thickness in plumbago crucible, after the C/C matrix material sanding and polishing that band is connected cleaning, drying, put on it, then another part being laid in to (its thickness is with being about equally 4cm) on C/C matrix material, even if C/C matrix material is embedded in mixed powder; Then plumbago crucible is placed in to vacuum high-temperature Reaktionsofen, using argon gas as shielding gas, with the heat-up rate of 10 DEG C/min by furnace temperature to 2200 DEG C, insulation 2h, powered-down naturally cools to room temperature by it subsequently, obtains the C/C matrix material sample with SiC transition layer;
Step 3: take respectively massfraction and be 13% Li
2cO
3powder, 10% Al
2o
3powder, 75% SiO
2powder, is incubated 5h by these powders with putting into the oxidized still that corundum crucible is built in 1500 DEG C after ball mill mixing and ball milling 2h, carries out at once shrend after taking-up, obtains LAS glass block; Then oven dry, fragmentation then, after wet-milling (taking distilled water as medium) 11h, dried 36h in 100 DEG C of baking ovens, crosses 300 mesh sieves, finally obtains LAS glass powder for subsequent use;
When preparation LAS glass powder, add micro-TiO
2, B
2o
3and Sb
2o
3powder.
Step 4: taking respectively massfraction is 17% ZnO powder, 15% Al
2o
3powder, 64% SiO
2powder, 4%TiO
2powder and 0.5%Sb
2o
3, these powders are incubated to 5h with putting into the oxidized still that corundum crucible is built in 1550 DEG C after ball mill ball milling mixing 1.5h, after taking-up, carry out at once shrend, obtain ZAS glass block; Then oven dry, fragmentation then dried 36h after wet-milling (taking distilled water as medium) 11h in 100 DEG C of baking ovens, crosses 300 mesh sieves, finally obtains ZAS glass powder for subsequent use;
Step: 5: take the ZAS glass powder 2g and the 2ml dehydrated alcohol that are obtained by step 4, both are mixed and made into serum, then brush on the C/C matrix material specimen surface with SiC transition layer of being prepared by step 2 (being face to be connected), be then placed in 80 DEG C of baking ovens and dry 30min; After oven dry, be placed in the hot pressing die of high-strength graphite material, more prepared LAS glass powder 18g is poured on it and tiled evenly, then grinding tool is put into vacuum hotpressing stove;
Step 6: first to hot pressing furnace extracting vacuum, below being extracted into negative pressure time, with 5 DEG C/min heat-up rate, furnace temperature is risen to 1225 DEG C from room temperature again, insulation 30min also loads 25MPa pressure, after finishing, insulation closes heating power supply with stove naturally cooling, release in the time that temperature drops to 1000 DEG C, the sample that is processed into 12mm × 8mm × 6mm that takes out while continuing to be cooled to room temperature to be cooled does the shearing test under room temperature.Shearing test result shows, prepared joint average shear intensity is 28.63MPa.
Embodiment 3:
Step 1: the C/C matrix material of processed 30mm × 30mm × 4mm is put into dehydrated alcohol ultrasonic cleaning, be then placed in baking oven dry for standby at 100 DEG C;
Step 2: take respectively massfraction and be 75% Si powder, 20% C powder and 5% Al
2o
3powder, takes out these three kinds of powders with ball mill mixing and ball milling 2h, be then placed in baking oven 30min at 100 DEG C and dry; A dry blending powder part for preparation is first encased in to about 4cm thickness in plumbago crucible, after the C/C matrix material sanding and polishing that band is connected cleaning, drying, put on it, then another part being laid in to (its thickness is with being about equally 4cm) on C/C matrix material, even if C/C matrix material is embedded in mixed powder; Then plumbago crucible is placed in to vacuum high-temperature Reaktionsofen, using argon gas as shielding gas, with the heat-up rate of 10 DEG C/min by furnace temperature to 2100 DEG C, insulation 2h, powered-down naturally cools to room temperature by it subsequently, obtains the C/C matrix material sample with SiC transition layer;
Step 3: take respectively massfraction and be 16% Li
2cO
3powder, 13% Al
2o
3powder, 70% SiO
2powder, is incubated 5h by these powders with putting into the oxidized still that corundum crucible is built in 1550 DEG C after ball mill mixing and ball milling 2h, carries out at once shrend after taking-up, obtains LAS glass block; Then oven dry, fragmentation then, after wet-milling (taking distilled water as medium) 11h, dried 48h in 100 DEG C of baking ovens, crosses 300 mesh sieves, finally obtains LAS glass powder for subsequent use;
When preparation LAS glass powder, add micro-TiO
2, B
2o
3and Sb
2o
3powder.
Step 4: taking respectively massfraction is 19% ZnO powder, 12% Al
2o
3powder, 65% SiO
2powder, 3%TiO2 powder and 0.5%Sb
2o
3, these powders are incubated to 5h with putting into the oxidized still that corundum crucible is built in 1550 DEG C after ball mill ball milling mixing 1.5h, after taking-up, carry out at once shrend, obtain ZAS glass block; Then oven dry, fragmentation then dried 48h after wet-milling (taking distilled water as medium) 11h in 100 DEG C of baking ovens, crosses 300 mesh sieves, finally obtains ZAS glass powder for subsequent use;
Step: 5: take the ZAS glass powder 1.5g and the 1.5ml dehydrated alcohol that are obtained by step 4, both are mixed and made into serum, then brush on the C/C matrix material specimen surface with SiC transition layer of being prepared by step 2 (being face to be connected), be then placed in 90 DEG C of baking ovens and dry 30min; After oven dry, be placed in the hot pressing die of high-strength graphite material, more prepared LAS glass powder 18g is poured on it and tiled evenly, then grinding tool is put into vacuum hotpressing stove;
Step 6: first to hot pressing furnace extracting vacuum, below being extracted into negative pressure time, with 5 DEG C/min heat-up rate, furnace temperature is risen to 1200 DEG C from room temperature again, insulation 15min also loads 25MPa pressure, after finishing, insulation closes heating power supply with stove naturally cooling, release in the time that temperature drops to 1000 DEG C, the sample that is processed into 12mm × 8mm × 6mm that takes out while continuing to be cooled to room temperature to be cooled does the shearing test under room temperature.Shearing test result shows, prepared joint average shear intensity is 30.06MPa.
Be that prepared joint section S EM figure can find out that middle layer ZAS and SiC coating are in conjunction with tight from Fig. 1, interface is without obvious crackle and hole.SiC coating is combined closely with C/C matrix, and middle layer ZAS is combined well with LAS glass-ceramic, and both components are oozed mutually, without significantly interface boundary.Taking ZAS glass as intermediate connecting layer and under suitable hot pressing parameters, the C/C of gained (SiC)/ZAS/LAS joint design is tight, and interface is in conjunction with good.Fig. 2 is the shearing area SEM picture of C/C-LAS joint and the XRD figure of section spectrum, from then on figure can find out that C/C-LAS joint fracture surface under shearing force presents stepped, can see the unsticking of carbon fiber in subregion and extract, in addition its load-displacement curves is comparatively mild and have a repeatedly primary deflector, this is also with the unsticking of carbon fiber and extract consistently, and its effect is the intensity that has further improved joint.
Claims (9)
1. a method of preparing carbon/carbon compound material and lithium aluminosilicate glass ceramic joint, is characterized in that step is as follows:
Step 1: the Si powder that is 60～80% by massfraction, 15～25% C powder and 5～15% Al
2o
3powder mixing and ball milling 1～3h post-drying obtains mixed powder; Mixed powder is packed in plumbago crucible, and carbon/carbon compound material C/C is embedded in mixed powder; Then plumbago crucible is placed in to vacuum high-temperature Reaktionsofen, using argon gas as shielding gas, with the heat-up rate of 5～10 DEG C/min by furnace temperature to 2000～2200 DEG C, insulation 1～3h, powered-down naturally cools to room temperature by it subsequently, obtains the C/C matrix material with SiC transition layer; Described carbon/carbon compound material C/C is ultrasonic cleaning oven dry in dehydrated alcohol;
Step 2: ZAS glass powder is made to serum taking dehydrated alcohol as dispersant, and brushing, on to be connected of the C/C matrix material with SiC transition layer, is placed in 80～100 DEG C of baking ovens and dries.
Step 3: the C/C matrix material that step 2 is dried is placed in the hot pressing die of high-strength graphite material, pours LAS glass powder into be connected and goes up and tile evenly, then grinding tool is put into vacuum hotpressing stove;
Step 4: first to hot pressing furnace extracting vacuum, below being extracted into negative pressure time, with 5～10 DEG C/min heat-up rate, furnace temperature is risen to 1200～1300 DEG C from room temperature, insulation 15～45min also loads 20～25MPa pressure, after finishing, insulation closes heating power supply with stove naturally cooling, release in the time that temperature drops to 1000 DEG C, the carbon/carbon compound material-lithium aluminosilicate glass ceramic joint obtaining that takes out while continuing to be cooled to room temperature to be cooled.
2. the method for preparing according to claim 1 carbon/carbon compound material and lithium aluminosilicate glass ceramic joint, is characterized in that: the preparation of described ZAS glass powder: the Li that is 10～18% by massfraction
2cO
3powder, 10～20% Al
2o
3powder and 55～75% SiO
2powder, puts into the oxidized still that corundum crucible is built in 1500～1600 DEG C and is incubated 3～5h after mixing and ball milling 1～3h, carry out at once shrend after taking-up, obtains LAS glass block; Then by LAS glass block crushing drying, taking distilled water as medium wet-milling 9～11h post-drying, cross 300 mesh sieves, finally obtain LAS glass powder.
3. the method for preparing according to claim 1 carbon/carbon compound material and lithium aluminosilicate glass ceramic joint, is characterized in that: the preparation of described ZAS glass powder: the ZnO powder that is 15～25% by massfraction, 10～20% Al
2o
3powder, 60～75% SiO
2powder, 2～5% TiO
2powder and 0.5% Sb
2o
3, ball milling mixes to be put into the oxidized still that corundum crucible is built in 1500～1600 DEG C after 1～3h and is incubated 3～5h, carries out at once shrend after taking-up, obtains ZAS glass block; Then by ZAS glass block crushing drying, taking distilled water as medium wet-milling 9～11h post-drying, cross 300 mesh sieves, finally obtain ZAS glass powder.
4. the method for preparing according to claim 2 carbon/carbon compound material and lithium aluminosilicate glass ceramic joint, is characterized in that: when preparation LAS glass powder, add micro-TiO
2, B
2o
3and Sb
2o
3powder.
5. the method for preparing according to claim 1 carbon/carbon compound material and lithium aluminosilicate glass ceramic joint, is characterized in that: described C powder and Si powder purity are 99%, and granularity is 300 orders.
6. the method for preparing according to claim 2 carbon/carbon compound material and lithium aluminosilicate glass ceramic joint, is characterized in that: described Li
2cO
3powder, Al
2o
3powder and SiO
2powder is analytical pure, and purity is not less than 97%, and granularity is 300 orders.
7. the method for preparing according to claim 3 carbon/carbon compound material and lithium aluminosilicate glass ceramic joint, is characterized in that: described ZnO powder, Al
2o
3powder, SiO
2powder, TiO
2powder and Sb
2o
3be analytical pure, purity is not less than 97%, and granularity is 300 orders.
8. the method for preparing according to claim 4 carbon/carbon compound material and lithium aluminosilicate glass ceramic joint, is characterized in that: described TiO
2, B
2o
3and Sb
2o
3powder is analytical pure, and purity is not less than 97%, and granularity is 300 orders.
9. the method for preparing according to claim 1 carbon/carbon compound material and lithium aluminosilicate glass ceramic joint, is characterized in that: the negative pressure state of described step 4 is furnace pressure ∠ 10
-1pa.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518129A (en) * | 2016-11-03 | 2017-03-22 | 西北工业大学 | Method for promoting shearing performance of carbon/carbon-lithium aluminum silicon joint |
| 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 |
| CN112299869A (en) * | 2020-10-28 | 2021-02-02 | 中国科学院上海硅酸盐研究所 | Laser welding method for silicon carbide and composite material thereof |
| CN114804626A (en) * | 2022-04-11 | 2022-07-29 | 哈尔滨工业大学（威海） | Li-B-Si-Al-O glass system wave-transparent hydrophobic coating and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232256A (en) * | 2013-03-01 | 2013-08-07 | 西北工业大学 | Method for improving connection performances of C/C composite material-Li-Al-Si ceramic joint |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232256A (en) * | 2013-03-01 | 2013-08-07 | 西北工业大学 | Method for improving connection performances of C/C composite material-Li-Al-Si ceramic joint |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518129A (en) * | 2016-11-03 | 2017-03-22 | 西北工业大学 | Method for promoting shearing performance of carbon/carbon-lithium aluminum silicon joint |
| 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 |
| CN112299869A (en) * | 2020-10-28 | 2021-02-02 | 中国科学院上海硅酸盐研究所 | Laser welding method for silicon carbide and composite material thereof |
| CN114804626A (en) * | 2022-04-11 | 2022-07-29 | 哈尔滨工业大学（威海） | Li-B-Si-Al-O glass system wave-transparent hydrophobic coating and preparation method thereof |
| CN114804626B (en) * | 2022-04-11 | 2023-06-02 | 哈尔滨工业大学（威海） | Li-B-Si-Al-O glass system wave-transparent hydrophobic coating and preparation method thereof |
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