CN104529501A - Binder for bonding insulating materials to surfaces of SiC-based fibrous composites and application method thereof - Google Patents

Binder for bonding insulating materials to surfaces of SiC-based fibrous composites and application method thereof Download PDF

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CN104529501A
CN104529501A CN201510015127.5A CN201510015127A CN104529501A CN 104529501 A CN104529501 A CN 104529501A CN 201510015127 A CN201510015127 A CN 201510015127A CN 104529501 A CN104529501 A CN 104529501A
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powder
sio
mixed powder
sintering
adhesive layer
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CN104529501B (en
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丁万昱
刘金东
崔云先
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Dalian Jiaotong University
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Abstract

The invention relates to a binder for bonding insulating materials to surfaces of SiC-based fibrous composites and an application method of the binder, and belongs to the field of surface machining and coatings. The binder is composed of Ca2SiO4 powder, Na2SiO3 powder and SiO2 powder, and the molar ratio of the Ca2SiO4 powder, the Na2SiO3 powder and the SiO2 powder is 3 to 1:2:4:16. The binder has the advantages that binder layers of different coefficients of thermal expansion are prepared by adjusting the molar ratio of the Ca2SiO4 powder, the Na2SiO3 powder and the SiO2 powder, and good bonding performance between the binder and the surfaces of the SiC-based fibrous composites and between the binder and the surfaces of the insulating materials is achieved.

Description

A kind of binding agent at SiC base fibre composite surface adhesion insulating material and using method thereof
Technical field
The present invention relates to a kind of binding agent at SiC base fibre composite surface adhesion insulating material and using method thereof, belong to surface working and coatings art.
Background technology
SiC base fibre composite, as carbon fiber-reinforced SiC material, the fiber reinforced SiC material of SiC etc., be the important functional materials of a class, have important application at aerospace field, as the thermal protective system etc. of aircraft engine, rocket engine and re-entry space vehicle.In recent years, the inefficacy of SiC base fibre composite under rapid temperature rise and drop condition characterizes the concern more and more causing people, as the instantaneous temperature, instantaneous strain etc. of SiC base fibre composite in test rapid temperature rise and drop process.The method of test material temperature has hot resistance method, thermocouple method, IR thermometry etc.; The method of test strain has electrometric method, flash spotting, mechanical survey method etc.Consider the applied environment of SiC base fibre composite at the narrow and small high temperature of aerospace field, and instantaneous temperature, instantaneous strain test request, film thermocouple temp measuring method and sheet resistance strain testing method become the instantaneous temperature of SiC base fibre composite in rapid temperature rise and drop process, the best testing method of instantaneous strain.But due to the interlaced loose and porous structure of SiC base fibre composite micron order, its micron order hole can cause the functional layer defect of thin film thermoelectric even summation sheet resistance strainometer; Due to SiC base fibre composite micron order braiding structure, under varying temperature environment, fibrous texture displacement is caused to destroy the functional layer of thin film thermoelectric even summation sheet resistance strainometer by thermal expansion; Because the electrical properties of SiC base fibre composite is better, short circuit between the functional layer of thin film thermoelectric even summation sheet resistance strainometer and SiC base fibre composite can be caused.For these reasons, need at the SiC base fibre composite surface insulation layer that first preparation is fine and close continuously, prepare the functional layer of thin film thermoelectric even summation sheet resistance strainometer more on the insulating layer, realize the test to SiC base fibre composite instantaneous temperature, instantaneous strain.
At present, prepared by SiC base fibre composite surface to the method for coating/thin film has the people such as X.Yin (MaterialsScience & Engineering A, 2000, Vol.290:89-94) to propose with CrO 3, H 2sO 4for the CrSi permeating method of raw material; The people such as F.Smeacetto (Carbon, 2002, Vol.40:583-587) propose with Y 2o 3, BC, BaBSiO xfor the direct reaction method of raw material; F. deng people (Surface & Coatings Technology, 2008, Vol.202:1588-1593) propose with SiC+SiO 2or SiC+Si is the lf method of raw material; The people such as F.Smeacetto (Ceramics International, 2008, Vol.34:1297-1301) propose with Si, SiO 2, Al 2o 3, Y 2o 3for the high temperature sintering methods of raw material; The Direct Laser irradiance method that the people such as S.Costil (Applied Surface Science, 2008, Vol.255:2425-2432) propose; The people (Surface & Coatings Technology, 2012, Vol.206:4166-4172) such as Patrick Ritt propose with Mo (CO) 6, the powder such as Si, B is the sintering method of raw material; The people such as X.Yang (Vacuum, 2013, Vol.96:63-68) propose with Zr, Si, PCS-DVB, Al 2o 3be the sintering method of raw material Deng powder; The people such as M.Albano (Acta Astronautica, 2014, Vol.99:276-282) propose with CH 3siCl, CH 3siCl 3for the chemical meteorology deposition method of raw material; The people such as Y.P.Xie (Ceramics International, 2014, Vol.40:6875-6880) propose with C 3h 6, CH 3siCl 3, H 2, Ar is the chemical vapor infiltration method etc. of raw material.
Aforesaid method all comes with some shortcomings part, e.g., if prepare coating/thin film with chemical vapor infiltration method, then there is temperature of reaction too high, destructible SiC base fibre composite, simultaneously the problem such as long, inefficiency consuming time; If prepare coating/thin film with direct sintering method, then there is the problems such as sintering temperature is too high, destructible SiC base fibre composite; If prepare coating/thin film with laser irradiating method, then there is the problems such as laser beam spot is little, inefficiency, irradiation surface difficult control of temperature; If prepare coating/thin film with powder sintering method method, then have that coating/thin film surfaceness is excessive, coatingsurface exists the problems such as a large amount of random cracks.
Summary of the invention
The present invention passes through with Ca 2siO 4powder, Na 2siO 3powder and SiO 2powder is the sintering method of raw material, solves the problems referred to above.
The invention provides a kind of binding agent in SiC base fibre composite cohesive insulation material on the surface, described binding agent is by Ca 2siO 4powder, Na 2siO 3powder and SiO 2powder constituent, described Ca 2siO 4powder, Na 2siO 3powder and SiO 2the mol ratio of powder is 3 ~ 12:4:16.
SiC base fibre composite of the present invention is preferably carbon fiber-reinforced SiC material of the prior art, the fiber reinforced SiC material of SiC, carbon fiber-reinforced Si 3n 4material, carbon fiber-reinforced CN material, the fiber reinforced Si of SiC 3n 4material and the fiber reinforced CN material of SiC etc.
Insulating material of the present invention is preferably quartz plate, alumina wafer and sheet mica etc., and described insulation thickness is preferably >=500 μm.
Another object of the present invention utilizes above-mentioned binding agent in the method for SiC base fibre composite cohesive insulation material on the surface, and described method comprises the steps:
When adhesive layer is individual layer:
By Ca 2siO 4powder, Na 2siO 3powder and SiO 2massage that, than being 3 ~ 12:4:16 mixing, obtaining mixed powder, mixed powder is placed in SiC base fibre composite on the surface, is placed in by insulating material on mixed powder, and sintering, is cooled to room temperature;
When adhesive layer is multilayer:
1. by Ca 2siO 4powder, Na 2siO 3powder and SiO 2massage that, than being 3 ~ 12:4:16 mixing, obtains mixed powder;
2. the mixed powder of step 1. gained is placed in SiC base fibre composite on the surface, sintering, is cooled to room temperature;
3. 1. repeating step operates, and the mixed powder this step obtained is placed on the adhesive layer of previous step products obtained therefrom, and sintering, is cooled to room temperature;
4. 3. repeating step operates, and obtains multi-layered bonded oxidant layer, and the last time during sintered bond oxidant layer, be placed in by insulating material on the mixed powder of last preparation, sintering, is cooled to room temperature.
The present invention is by regulating Ca 2siO 4powder, Na 2siO 3powder and SiO 2the mol ratio of powder, prepare the adhesive layer with different heat expansion coefficient, make the junction of adhesive layer and SiC base fibre composite have the thermal expansivity close with SiC base fibre composite, also make the junction of adhesive layer and insulating material have the thermal expansivity close with insulating material simultaneously.
Married operation of the present invention is preferably Ca 2siO 4powder, Na 2siO 3powder, SiO 2powder and water for ball milling, drying.
Ball-milling Time of the present invention is preferably 10 ~ 600min.
The overlay capacity of mixed powder of the present invention on SiC base fibre composite surface is preferably 0.01 ~ 0.2g/cm 2.
The overlay capacity of mixed powder of the present invention on adhesive layer is preferably 0.01 ~ 0.2g/cm 2.
Sintering temperature of the present invention is preferably 950 ~ 1100 DEG C.
Sintering time of the present invention is preferably 30 ~ 120min.
Method of cooling of the present invention is preferably at the uniform velocity cooled to the temperature fall time >=12h of 100 DEG C from sintering temperature, be at the uniform velocity cooled to the temperature fall time >=1h of room temperature from 100 DEG C.
Beneficial effect of the present invention is:
1. the present invention is by regulating Ca 2siO 4powder, Na 2siO 3powder and SiO 2the mol ratio of powder, prepares the adhesive layer with different heat expansion coefficient, and forms good adhesive property with SiC base fibre composite surface and insulating material surface;
2. adhesive layer of the present invention can resistance to temperatures as high 800 DEG C;
3. mixed powder of the present invention is not containing organism, sulfide, nitride and fluorochemical etc., do not produce pollution in sintering process, without the need to aftertreatment after sintering, directly can prepare thin film thermoelectric occasionally sheet resistance strainometer etc. on the insulating material;
4. the present invention can also utilize binding agent of the present invention to bond the functional materials of other character at SiC base fibre composite on the surface;
5. adhesive method of the present invention is simple, with low cost, the sintering period is short, sintering process is easy to control, productive rate is high, be convenient to large-scale industrial production.
Accompanying drawing explanation
Accompanying drawing 9 width of the present invention,
Fig. 1 is the cross section structure schematic diagram of product prepared by embodiment 1 ~ 5;
Fig. 2 be embodiment 1 prepare the adhesive layer of product and the cross section, junction of carbon fiber-reinforced SiC material amplify 100 times of SEM shape appearance figures;
Fig. 3 be embodiment 1 prepare the adhesive layer of product and the cross section, junction of carbon fiber-reinforced SiC material amplify 500 times of SEM shape appearance figures;
Fig. 4 be embodiment 1 prepare the adhesive layer of product and the cross section, junction of quartz plate amplify 10000 times of SEM shape appearance figures;
Fig. 5 be embodiment 1 prepare the adhesive layer of product and the cross section, junction of quartz plate amplify 20000 times of SEM shape appearance figures;
Fig. 6 be embodiment 2 prepare the adhesive layer of product and the cross section, junction of carbon fiber-reinforced SiC material amplify 500 times of SEM shape appearance figures;
Fig. 7 be embodiment 3 prepare the adhesive layer of product and the cross section, junction of carbon fiber-reinforced SiC material amplify 500 times of SEM shape appearance figures;
Fig. 8 be embodiment 4 prepare the adhesive layer of product and the cross section, junction of carbon fiber-reinforced SiC material amplify 500 times of SEM shape appearance figures;
Fig. 9 be embodiment 5 prepare the adhesive layer of product and the cross section, junction of carbon fiber-reinforced SiC material amplify 500 times of SEM shape appearance figures;
Wherein, 1, quartz plate, 2, adhesive layer, 3, carbon fiber-reinforced SiC material.
Embodiment
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
Embodiment 1
Bond in carbon fiber-reinforced SiC material the method for quartz plate on the surface, and described method comprises the steps:
1. by Ca 2siO 4powder, Na 2siO 3powder and SiO 2your ratio of massage is 3:4:16 mixing, add deionized water and form slurry, be placed in ball grinder, utilize tumbling ball mill that slurry is carried out ball milling, ball milling speed is 30r/min, and Ball-milling Time is 10h, ball milling is placed on 50 DEG C of dry 4h in baking oven, obtain mixed powder I, mixed powder I is laid in carbon fiber-reinforced SiC material on the surface, the overlay capacity of mixed powder I on carbon fiber-reinforced SiC material surface is 0.03g/cm 2be placed in 1100 DEG C of sintering 60min in retort furnace, mixed powder I sinters rear formation adhesive layer I, and the temperature fall time being at the uniform velocity cooled to 100 DEG C from sintering temperature is 20h, the temperature fall time being at the uniform velocity cooled to room temperature from 100 DEG C is 1h, by smooth for adhesive layer I surface grinding;
2. by Ca 2siO 4powder, Na 2siO 3powder and SiO 2your ratio of massage is 7:4:16 mixing, add deionized water and form slurry, be placed in ball grinder, utilize tumbling ball mill that slurry is carried out ball milling, ball milling speed is 30r/min, and Ball-milling Time is 12h, ball milling is placed on 50 DEG C of dry 4h in baking oven, obtain mixed powder II, be laid in by mixed powder II on adhesive layer I, the overlay capacity of mixed powder II on adhesive layer I is 0.03g/cm 2be placed in 1100 DEG C of sintering 60min in retort furnace, mixed powder II sinters rear formation adhesive layer II, and the temperature fall time being at the uniform velocity cooled to 100 DEG C from sintering temperature is 20h, the temperature fall time being at the uniform velocity cooled to room temperature from 100 DEG C is 1h, by smooth for adhesive layer II surface grinding;
3. by Ca 2siO 4powder, Na 2siO 3powder and SiO 2your ratio of massage is 12:4:16 mixing, add deionized water and form slurry, be placed in ball grinder, utilize tumbling ball mill that slurry is carried out ball milling, ball milling speed is 30r/min, and Ball-milling Time is 16h, ball milling is placed on 50 DEG C of dry 4h in baking oven, obtain mixed powder III, be laid in by mixed powder III on adhesive layer II, the overlay capacity of mixed powder III on adhesive layer II is 0.03g/cm 2, be placed on mixed powder III by 500 μm of thick quartz plates, be placed in 950 DEG C of sintering 60min in retort furnace, the temperature fall time being at the uniform velocity cooled to 100 DEG C from sintering temperature is 20h, and the temperature fall time being at the uniform velocity cooled to room temperature from 100 DEG C is 1h.
Embodiment 2
Bond in carbon fiber-reinforced SiC material the method for quartz plate on the surface, and described method comprises the steps:
1. by Ca 2siO 4powder, Na 2siO 3powder and SiO 2your ratio of massage is 3:4:16 mixing, add deionized water and form slurry, be placed in ball grinder, utilize tumbling ball mill that slurry is carried out ball milling, ball milling speed is 30r/min, and Ball-milling Time is 12h, ball milling is placed on 50 DEG C of dry 4h in baking oven, obtain mixed powder I, mixed powder I is laid in carbon fiber-reinforced SiC material on the surface, the overlay capacity of mixed powder I on carbon fiber-reinforced SiC material surface is 0.04g/cm 2be placed in 1100 DEG C of sintering 60min in retort furnace, mixed powder I sinters rear formation adhesive layer I, and the temperature fall time being at the uniform velocity cooled to 100 DEG C from sintering temperature is 22h, the temperature fall time being at the uniform velocity cooled to room temperature from 100 DEG C is 1h, by smooth for adhesive layer I surface grinding;
2. by Ca 2siO 4powder, Na 2siO 3powder and SiO 2your ratio of massage is 12:4:16 mixing, add deionized water and form slurry, be placed in ball grinder, utilize tumbling ball mill that slurry is carried out ball milling, ball milling speed is 30r/min, and Ball-milling Time is 14h, ball milling is placed on 50 DEG C of dry 4h in baking oven, obtain mixed powder II, be laid in by mixed powder II on adhesive layer I, the overlay capacity of mixed powder II on adhesive layer I is 0.03g/cm 2, be placed on mixed powder II by 500 μm of thick quartz plates, be placed in 950 DEG C of sintering 60min in retort furnace, the temperature fall time being at the uniform velocity cooled to 100 DEG C from sintering temperature is 20h, and the temperature fall time being at the uniform velocity cooled to room temperature from 100 DEG C is 1h.
Embodiment 3
Bond in carbon fiber-reinforced SiC material the method for quartz plate on the surface, and described method comprises the steps:
1. by Ca 2siO 4powder, Na 2siO 3powder and SiO 2your ratio of massage is 3:4:16 mixing, add deionized water and form slurry, be placed in ball grinder, utilize planetary ball mill that slurry is carried out ball milling, ball milling speed is 400r/min, and Ball-milling Time is 2h, ball milling is placed on 50 DEG C of dry 4h in baking oven, obtain mixed powder I, mixed powder I is laid in carbon fiber-reinforced SiC material on the surface, the overlay capacity of mixed powder I on carbon fiber-reinforced SiC material surface is 0.04g/cm 2be placed in 1100 DEG C of sintering 60min in retort furnace, mixed powder I sinters rear formation adhesive layer I, and the temperature fall time being at the uniform velocity cooled to 100 DEG C from sintering temperature is 20h, the temperature fall time being at the uniform velocity cooled to room temperature from 100 DEG C is 1h, by smooth for adhesive layer I surface grinding;
2. by Ca 2siO 4powder, Na 2siO 3powder and SiO 2your ratio of massage is 11:4:16 mixing, add deionized water and form slurry, be placed in ball grinder, utilize planetary ball mill that slurry is carried out ball milling, ball milling speed is 400r/min, and Ball-milling Time is 4h, ball milling is placed on 50 DEG C of dry 4h in baking oven, obtain mixed powder II, be laid in by mixed powder II on adhesive layer I, the overlay capacity of mixed powder II on adhesive layer I is 0.03g/cm 2, be placed on mixed powder II by 500 μm of thick quartz plates, be placed in 950 DEG C of sintering 60min in retort furnace, the temperature fall time being at the uniform velocity cooled to 100 DEG C from sintering temperature is 18h, and the temperature fall time being at the uniform velocity cooled to room temperature from 100 DEG C is 1h.
Embodiment 4
Bond in carbon fiber-reinforced SiC material the method for quartz plate on the surface, and described method comprises the steps:
1. by Ca 2siO 4powder, Na 2siO 3powder and SiO 2your ratio of massage is 3:4:16 mixing, add deionized water and form slurry, be placed in ball grinder, utilize planetary ball mill that slurry is carried out ball milling, ball milling speed is 400r/min, and Ball-milling Time is 2h, ball milling is placed on 50 DEG C of dry 4h in baking oven, obtain mixed powder I, mixed powder I is laid in carbon fiber-reinforced SiC material on the surface, the overlay capacity of mixed powder I on carbon fiber-reinforced SiC material surface is 0.04g/cm 2be placed in 1100 DEG C of sintering 60min in retort furnace, mixed powder I sinters rear formation adhesive layer I, and the temperature fall time being at the uniform velocity cooled to 100 DEG C from sintering temperature is 22h, the temperature fall time being at the uniform velocity cooled to room temperature from 100 DEG C is 1h, by smooth for adhesive layer I surface grinding;
2. by Ca 2siO 4powder, Na 2siO 3powder and SiO 2your ratio of massage is 10:4:16 mixing, add deionized water and form slurry, be placed in ball grinder, utilize planetary ball mill that slurry is carried out ball milling, ball milling speed is 400r/min, and Ball-milling Time is 4h, ball milling is placed on 50 DEG C of dry 4h in baking oven, obtain mixed powder II, be laid in by mixed powder II on adhesive layer I, the overlay capacity of mixed powder II on adhesive layer I is 0.03g/cm 2, be placed on mixed powder II by 500 μm of thick quartz plates, be placed in 950 DEG C of sintering 60min in retort furnace, the temperature fall time being at the uniform velocity cooled to 100 DEG C from sintering temperature is 20h, and the temperature fall time being at the uniform velocity cooled to room temperature from 100 DEG C is 1h.
Embodiment 5
Bond in carbon fiber-reinforced SiC material the method for quartz plate on the surface, and described method comprises the steps:
By Ca 2siO 4powder, Na 2siO 3powder and SiO 2your ratio of massage is 12:4:16 mixing, add deionized water and form slurry, be placed in ball grinder, utilize tumbling ball mill that slurry is carried out ball milling, ball milling speed is 30r/min, and Ball-milling Time is 12h, ball milling is placed on 50 DEG C of dry 4h in baking oven, obtain mixed powder, mixed powder is laid in carbon fiber-reinforced SiC material on the surface, the overlay capacity of mixed powder on carbon fiber-reinforced SiC material surface is 0.15g/cm 2, be placed on mixed powder by quartz plate thick for 1mm, be placed in 950 DEG C of sintering 120min in retort furnace, the temperature fall time being at the uniform velocity cooled to 100 DEG C from sintering temperature is 18h, and the temperature fall time being at the uniform velocity cooled to room temperature from 100 DEG C is 1h.

Claims (8)

1., at a binding agent for SiC base fibre composite cohesive insulation material on the surface, it is characterized in that: described binding agent is by Ca 2siO 4powder, Na 2siO 3powder and SiO 2powder constituent, described Ca 2siO 4powder, Na 2siO 3powder and SiO 2the mol ratio of powder is 3 ~ 12:4:16.
2. utilize binding agent described in claim 1 in a method for SiC base fibre composite cohesive insulation material on the surface, it is characterized in that: described method comprises the steps:
When adhesive layer is individual layer:
By Ca 2siO 4powder, Na 2siO 3powder and SiO 2massage that, than being 3 ~ 12:4:16 mixing, obtaining mixed powder, mixed powder is placed in SiC base fibre composite on the surface, is placed in by insulating material on mixed powder, and sintering, is cooled to room temperature;
When adhesive layer is multilayer:
1. by Ca 2siO 4powder, Na 2siO 3powder and SiO 2massage that, than being 3 ~ 12:4:16 mixing, obtains mixed powder;
2. the mixed powder of step 1. gained is placed in SiC base fibre composite on the surface, sintering, is cooled to room temperature;
3. 1. repeating step operates, and the mixed powder this step obtained is placed on the adhesive layer of previous step products obtained therefrom, and sintering, is cooled to room temperature;
4. 3. repeating step operates, and obtains multi-layered bonded oxidant layer, and the last time during sintered bond oxidant layer, be placed in by insulating material on the mixed powder of last preparation, sintering, is cooled to room temperature.
3. method according to claim 2, is characterized in that: described married operation is by Ca 2siO 4powder, Na 2siO 3powder, SiO 2powder and water for ball milling, drying.
4. method according to claim 2, is characterized in that: the overlay capacity of described mixed powder on SiC base fibre composite surface is 0.01 ~ 0.2g/cm 2.
5. method according to claim 2, is characterized in that: the overlay capacity of described mixed powder on adhesive layer is 0.01 ~ 0.2g/cm 2.
6. method according to claim 2, is characterized in that: described sintering temperature is 950 ~ 1100 DEG C.
7. method according to claim 2, is characterized in that: described sintering time is 30 ~ 120min.
8. method according to claim 2, is characterized in that: described method of cooling is at the uniform velocity be cooled to the temperature fall time >=12h of 100 DEG C from sintering temperature, is at the uniform velocity cooled to the temperature fall time >=1h of room temperature from 100 DEG C.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86100240A (en) * 1986-01-07 1987-07-22 中国有色金属工业总公司昆明贵金属研究所 Pottery-platinum composite crucible and manufacture method thereof
US6316048B1 (en) * 1999-12-20 2001-11-13 General Electric Company Methods for providing ceramic matrix composite components with increased thermal capacity
JP2006196674A (en) * 2005-01-13 2006-07-27 Kyocera Corp Method of manufacturing wiring board
CN101967313A (en) * 2010-11-03 2011-02-09 重庆国际复合材料有限公司 Protective coating for inhibiting platinum bushing from being oxidized and volatilized, and manufacturing method and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86100240A (en) * 1986-01-07 1987-07-22 中国有色金属工业总公司昆明贵金属研究所 Pottery-platinum composite crucible and manufacture method thereof
US6316048B1 (en) * 1999-12-20 2001-11-13 General Electric Company Methods for providing ceramic matrix composite components with increased thermal capacity
JP2006196674A (en) * 2005-01-13 2006-07-27 Kyocera Corp Method of manufacturing wiring board
CN101967313A (en) * 2010-11-03 2011-02-09 重庆国际复合材料有限公司 Protective coating for inhibiting platinum bushing from being oxidized and volatilized, and manufacturing method and application thereof

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