CN106141507B - A kind of preparation method of the ceramic granule reinforced composite material film of low content of organics - Google Patents
A kind of preparation method of the ceramic granule reinforced composite material film of low content of organics Download PDFInfo
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- CN106141507B CN106141507B CN201610514687.XA CN201610514687A CN106141507B CN 106141507 B CN106141507 B CN 106141507B CN 201610514687 A CN201610514687 A CN 201610514687A CN 106141507 B CN106141507 B CN 106141507B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0255—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in welding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/16—Composite materials, e.g. fibre reinforced
- B23K2103/166—Multilayered materials
- B23K2103/172—Multilayered materials wherein at least one of the layers is non-metallic
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Abstract
The present invention relates to a kind of preparation methods of the ceramic granule reinforced composite material film of low content of organics, including：（1）Ceramic powder, metal-powder, dispersant and binder are uniformly dispersed in a solvent, obtain suspension slurry after ball milling, the percent by volume of the ceramic powder and metal-powder is（10%~30%）：（70%~90%）, the gross mass of the dispersant and binder is no more than the 6wt.% of ceramic powder, metal-powder and solvent gross mass；（2）The suspension slurry of gained is obtained into the ceramic granule reinforced composite material film of the low content of organics according to required thickness tape casting at drying after composite soldering film.The present invention has wide applicability, and the combination of various ceramic particles and metal-powder can be applied, have very strong application prospect.
Description
Technical field
The present invention relates to a kind of systems for the ceramic granule reinforced composite material film can be used for ceramics or solder bonding metal field
Preparation Method belongs to metal and Ceramic brazing field.
Background technology
Ceramic material is because of its good comprehensive performance, such as high temperature resistant, acid-alkali-corrosive-resisting, low-density, high intensity, in its people
It is had a wide range of applications in economic every profession and trade, but ceramic material is because it is difficult to prepare large scale and shape that itself technology, which limits,
Complicated component.In addition, the application demand that ceramics are connect with traditional metal materials is in the row such as space flight, vacuum electron device, automobile
Industry is also very extensive, therefore, is taken seriously by the ceramic joining technology of representative of soldering tech, but due to the ceramics as base material
Material and Physical Properties of Metallicmateriais difference are very big, and the coefficient of thermal expansion and elasticity modulus gap of the two are apparent, therefore in pricker
The linkage interface of postwelding will produce apparent residual stress, and residual stress can lead to jointing fracture failure, influence connector
It uses.In recent years, it is inspired by metal-base composites, low-expansion coefficient, high resiliency mould is added in traditional metal solder
The ceramic particle of amount reduces the coefficient of thermal expansion of metal solder, and the composite soldering to reduce connector residual stress becomes research
Hot spot, but the bonding strength of ceramic joint with connect that layer thickness is closely related, it is strong that blocked up articulamentum inevitably results in connector
Degree declines, and there are mainly two types of ceramic granule reinforced composite material preparation methods traditional at present, and one is dry-press processes, i.e., will pottery
Dry-pressing flakiness uses after porcelain particle is mixed with metal-powder, and the thickness of thin slice is generally in 0.2mm or more；Another kind be wet method at
Ceramic particle and metal-powder are made the slurry with certain viscosity, then slurry are coated on connector and is brazed by shape,
Although such method articulamentum thinner thickness, thickness can not be grasped definitely, it is difficult to ensure that the uniformity of coating layer thickness, operation
The experience of person plays critically important effect, in addition, the large amount of organic of wet-formed middle addition can be waved in subsequent brazing process
Hair, leaves certain hole, influences soldering strength.
Invention content
Various ceramic particles and metal-powder are generally applicable in view of the above-mentioned problems, the purpose of the present invention is to provide one kind
, thickness can be controlled, and add the preparation method of the seldom ceramic granule reinforced composite material film of content of organics.
On the one hand, the present invention provides a kind of preparation sides of the ceramic granule reinforced composite material film of low content of organics
Method, including：
(1) ceramic powder, metal-powder, dispersant and binder are uniformly dispersed in a solvent, are suspended after ball milling
The percent by volume of slurry material, the ceramic powder and metal-powder is (10%~30%)：(70%~90%), the dispersion
The gross mass of agent and binder is no more than the 6wt.% of ceramic powder, metal-powder and solvent gross mass；
(2) suspension slurry of gained is dried according to required thickness tape casting at after composite soldering film, is obtained described
The ceramic granule reinforced composite material film of low content of organics.
Preferably, step (1) includes：Ceramic powder, dispersant are dissolved in solvent, then gold is added in ball milling 8~16 hours
Belong to powder, ball milling 2~6 hours；Binder is finally added, ball milling 4~12 hours prepares the suspension slurry for tape casting
Material.
Preferably, the solid content of the suspension slurry is 22~30vol.%.
Preferably, the dispersant is castor oil phosphate ester or/and castor oil, addition is ceramic powder, metal powder
2~3wt.% of body and solvent gross mass.
Preferably, the binder is polyvinyl butyral, addition is that ceramic powder, metal-powder and solvent are total
2~3wt.% of quality.
Preferably, the solvent is 2- butanone or/and ethyl alcohol.
Preferably, the solvent is the mixed solution of 2- butanone and ethyl alcohol, wherein the mass ratio of 2- butanone and ethyl alcohol is (60
~70):(30~40).
Preferably, the average grain diameter of the ceramic powder is 5~20 μm, the average grain diameter of the metal-powder is 1~50 μ
m。
Preferably, the height of scraper is 50~200 μm in tape casting.
Preferably, the environment of the drying be vacuum degree be less than 1Pa, drying temperature be 50~60 DEG C, drying time be 5~
10 hours.
On the other hand, the present invention also provides a kind of ceramic granule reinforced composite material films of low content of organics.
The beneficial effects of the invention are as follows：
1, the present invention provides a kind of preparation sides for being generally applicable to be made of composite soldering ceramic particle and metal-powder
Method has wide applicability, the combination of various ceramic particles and metal-powder can be applied, before having very strong application
Scape；
2, the present invention, which provides ceramic granule reinforced composite material film prepared by preparation method, has good flexibility, can roll over
It folds and cuts into any shape without breakage, be very suitable for the solder attended operation of ceramic material and metal material；
3, the present invention provides ceramic granule reinforced composite material film prepared by preparation method, and content of organics is less than
6wt.%, and other than dispersant and binder, without other organic additives, such as plasticiser, in the articulamentum after soldering not
The defects of will appear the hole generated because organic matter volatilizees, crackle, is conducive to improve strength of joint.
Description of the drawings
Fig. 1 a are SiC prepared by embodiment 1P/ (Ag powder+Cu powder+Ti powder) composite soldering film outward appearance figure；
Fig. 1 b are SiC prepared by embodiment 1P/ (Ag powder+Cu powder+Ti powder) composite soldering film micro-structure diagram；
Fig. 2 is in embodiment 1 using the SiC preparedP/ (Ag powder+Cu powder+Ti powder) composite soldering film connects silicon carbide ceramics
Connector micro-structure diagram；
Fig. 3 is B prepared by embodiment 24CP/ (Ag-Cu-Ti ternary alloy three-partalloys powder) composite soldering film outward appearance figure and microstructure
Figure；
Fig. 4 is the B prepared in embodiment 24CP/ (Ag-Cu-Ti ternary alloy three-partalloys powder) composite soldering film connects silicon carbide ceramics
Connector micro-structure diagram；
Fig. 5 is TiC prepared by embodiment 3P/ (Ni-Ti bianry alloys powder) composite soldering film outward appearance figure and micro-structure diagram.
Specific implementation mode
It is further illustrated the present invention below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
The present invention provides one kind low content of organics ceramics blanket to various ceramic particles and metal-powder
The preparation method of grain enhancing composite soldering film.The present invention uses tape casting technology, and it is multiple can to solve existing ceramic particle enhancing
It closes in solder technology of preparing, welding layer is blocked up and non-uniform disadvantage.The present invention by adding a small amount of dispersant and binder,
The content of organics for controlling composite soldering film simultaneously is less than 6wt.%, and the composite soldering film of preparation has good flexibility, micro-
Sight structure is uniform, is very suitable for low stresses, the high intensity soldering connection of ceramics and ceramics；If organic matter in composite soldering film
Too high levels, the defect formed in connector after brazing cause base material that can not form effective connection, therefore in latter embodiments
The comparative example of high content of organics composite soldering solder film connection is not provided.In addition, the composite soldering film toughness is fabulous, it can
To cut into any shape, be conducive to the practical operation of soldering connection, there is stronger practicability foreground.
It is the ceramic granule reinforced composite material film for illustratively illustrating low content of organics provided by the invention below
Preparation method.
Ceramic powder, metal-powder, dispersant and binder are uniformly dispersed in a solvent by a certain percentage, after ball milling
To suspension slurry.The gross mass of the wherein described dispersant and binder is no more than ceramic powder, metal-powder and the total matter of solvent
The 6wt.% of amount the defects of cavity, crackle can occurs to avoid articulamentum in subsequent brazing process, be conducive to improve soldering by force
Degree.Specifically, being gradually added ceramic powder, metal-powder, dispersant and binder etc. in such a way that substep is added can be with
The solid content of its suspension slurry is set to reach 22~30vol.%.As an example, ceramic powder, dispersant are dissolved in molten
Metal-powder, ball milling 2~6 hours (such as 4 hours) is then added in agent, ball milling 8~16 hours (such as 12 hours)；Finally again
Binder is added, ball milling 4~12 hours (such as 8 hours) prepares the suspension slurry for tape casting.
By the suspension slurry of gained according to required thickness tape casting at dry after composite soldering film, obtain described low having
The ceramic granule reinforced composite material film of machine object content.The height of scraper can be 50~200 μm wherein in tape casting, thus come
Control the thickness of the ceramic granule reinforced composite material film of the low content of organics.
In the above method, ceramic powder is chosen as the ceramic powder used in conventional solder, may be, for example, SiC, B4C、TiC、
Si3N4、TiB2Deng.Wherein, the percent by volume shared by ceramic powder can be ceramic powder and metal-powder total volume 10%~
30%.Metal powder can be two kinds or two or more metal-powder mixtures for having certain mixed proportion, can also be tool
The single atomization powder for having two-spot or the above ingredient of two-spot, may be, for example, Ag, Cu, Ti, Ni, Pd, In etc..The metal-powder institute
The percent by volume accounted for can be ceramic powder and metal-powder total volume 70%~90%.When choosing ceramics and metal-powder, pottery
The particle size range of porcelain particle can be 5~20 μm, and the particle size range of metal powder can be 1~50 μm, using ceramics as described above with
Metal powder material grain size is conducive to slurry viscosity and the control for being cast film thickness.
In the above method, dispersant can choose castor oil phosphate ester or/and castor oil.Its addition is ceramic powder, gold
Belong to 2~3wt.% of powder and solvent gross mass.
In the above method, the binder can be chosen for polyvinyl butyral, and addition to be used for tape casting
The viscosity of suspension slurry reach 1.5~4.0Pa.S, such as addition can be ceramic powder, metal-powder and solvent
2~3wt.% of gross mass.Suspension obtained by SR-5 type rheometers detection of the present invention using U.S.'s rheology Scientific Instruments Corporation
The viscosity of slurry.
In the above method, the solvent can be 2- butanone or/and ethyl alcohol, and addition is the suspension slurry for making to be formed
Solid content is 22~30vol.%22~30vol.%.Preferably, be 2- butanone and ethyl alcohol mixed solution, wherein 2- butanone and
The mass ratio of ethyl alcohol is (60~70):(30~40), such as 66:34.
In the above method, the environment of the drying can be that vacuum degree is less than 1Pa, and drying temperature can be 50~60 DEG C, dry
Time can be 5~10h.In the drying process, composite soldering film can be due to the volatilization of solvent so that its thickness reduces about 30-
40%, vacuum drying environment can ensure that the active metal in casting films avoids aoxidizing, and when suitable drying temperature and drying
Between can be shunk to avoid casting films and acutely lead to crackle, or be not achieved solvent volatilization temperature and dry and be not thorough.
Embodiment is enumerated further below so that the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary concrete numerical value.
Embodiment 1
Preparing the 20vol%SiC particles that thickness is 100~110 μm enhances (Ag powder+Cu powder+Ti powder) composite soldering film, step
It is rapid as follows：
(1) tape casting slurry solid content is 26vol.%, Ag powder：Cu powder：Ti powder=63wt.%:35.25wt.%:
1.75wt.%, SiC：(Ag powder+Cu powder+Ti powder)=20vol.%:80vol.%；Dispersant additive amount 3wt.%；Binder adds
Dosage 2.6wt.%；
(2) according to above-mentioned design proportion prepare 30g tape casting suspension slurries, weigh respectively 10 μm of SiC powder 1.8g,
Ag powder 13.66g, Cu powder 7.63g and Ti powder 0.38g, dispersant：Castor oil phosphate ester 0.9g, binder：Polyvinyl butyral
(PVB) 0.78g, solvent：2- butanone 4.31g, absolute ethyl alcohol 2.22g；
(3) SiC powder, dispersant and solvent are added in nylon crucible first, after sealing, 60g silicon carbide abrading-balls is added,
Batch mixing 12h on planetary batch mixer；Then, Ag powder, Cu powder and Ti powder are added in crucible together, after sealing, are continued in ball
Batch mixing 4h on grinding machine；Finally, binder is added in crucible, after sealing, batch mixing 8h, completion tape casting are outstanding again for all raw materials
The viscosity of the preparation of supernatant liquid slurry, the suspension slurry after preparation is 2.6Pa.S；
(4) suspension slurry is poured on surface to plate on the polyethylene film of silicon, scraper height is adjusted to 150 μm, along same
Slurry is equably cast on a carrier film by one direction；
(5) carrier film with casting films being placed in vacuum environment, vacuum degree is less than 1Pa, and drying temperature is 50 DEG C,
Drying time is 10h, between thickness is 100~110 μm after the casting films after drying are shunk.
Composite soldering film after drying is integrally removed from carrier silicon fiml, composite soldering film flexibility is very good, can be with
It arbitrarily folds and cuts, as shown in fig. la.Silicon-carbide particle and gold in composite soldering film are observed using scanning electron microscope
The distribution of metal particles, it can be found that silicon-carbide particle is evenly dispersed in Ag powder, Cu powder and Ti powder, as shown in Figure 1 b.
The joint geometry of composite soldering film as required after drying is cut, and using tooling in vacuum brazing
Implement soldering in stove.Microstructure such as Fig. 2 institutes of silicon carbide ceramics connector are connected using the composite soldering film of above-mentioned preparation
Show, it can be found that silicon-carbide particle is evenly dispersed in metal solder, entire connector is complete, and flawless, stomata etc. are any to be lacked
It falls into, the four-point bending intensity after connection can reach 275 ± 23MPa.
Embodiment 2
Prepare the 30vol.%B that thickness is 60~70 μm4C particles enhance Ag-Cu-Ti ternary alloy three-partalloy powder composite soldering films,
Steps are as follows：
(1) tape casting slurry solid content is 30vol.%, and ternary alloy three-partalloy powder is using atomization method, B4C：(A-
Cu-Ti)=30vol.%:70vol.%；Dispersant additive amount 3wt.%；Content of binder 3wt.%；
(2) 30g tape casting suspension slurries are prepared according to above-mentioned design proportion, weighs 5 μm of B respectively4C powder 2.36g,
Ag-Cu-Ti powder 21.27g, dispersant：Castor oil phosphate ester 0.9g, binder：Polyvinyl butyral (PVB) 0.9g, solvent：
2- butanone 4.20g, absolute ethyl alcohol 2.17g；
(3) first by B4C powder, dispersant and solvent are added in nylon crucible, and after sealing, 60g silicon carbide abrading-balls are added,
Batch mixing 12h on planetary batch mixer；Then, ternary Ag-Cu-Ti powder is added in crucible, after sealing, is continued on ball mill
Batch mixing 4h；Finally, binder is added in crucible, after sealing, all raw materials batch mixing 8h again completes tape casting suspension slurry
The viscosity of the preparation of material, the suspension slurry after preparation is 3.4Pa.S；
(4) suspension slurry is poured on surface to plate in the base vinyl film of silicon, scraper height is adjusted to 100 μm, along same
Slurry is equably cast on a carrier film by one direction；
(5) carrier film after curtain coating is placed in vacuum environment, vacuum degree is less than 1Pa, and drying temperature is 60 DEG C, dry
Time is 6h, between thickness is 60~70 μm after the casting films after drying are shunk.
Composite soldering film after drying is integrally removed from carrier silicon fiml, composite soldering film flexibility is very good, can be with
It arbitrarily folds and cuts, in Fig. 3 shown in (a).B in composite soldering film after drying4C even particulate dispersions are in ternary Ag-Cu-Ti
In metal-powder, in microstructure such as attached drawing 3 shown in (b).It can implement to be brazed after composite soldering film is cut.Using above-mentioned
The composite soldering film connection silicon carbide ceramics connector microstructure of preparation is as shown in figure 4, it can be found that connector is complete, zero defect,
Boron carbide particles concentrate on the intermediate zone of composite soldering, and the four-point bending intensity after connection can reach 236 ± 18MPa.
Embodiment 3
Preparing the 10vol.%TiC particles that thickness is 140~150 μm enhances Ni-Ti bianry alloy powder composite soldering films, step
It is rapid as follows：
(1) tape casting slurry solid content is 22vol.%, and ternary alloy three-partalloy powder is using atomization method, TiC：(Ni-
Ti)=10vol.%:90vol.%；Dispersant additive amount 3wt.%；Content of binder 3wt.%；
(2) according to above-mentioned design proportion prepare 30g tape casting suspension slurries, weigh respectively 20 μm of TiC powder 1.47g,
Ni-Ti powder 20.25g, dispersant：Castor oil 0.9g, binder：Polyvinyl butyral (PVB) 0.9g, solvent：2- butanone
5.46g, absolute ethyl alcohol 2.82g；
(3) TiC powder, dispersant and solvent are added in nylon crucible first, after sealing, 60g silicon carbide abrading-balls is added,
Batch mixing 12h on planetary batch mixer；Then, binary Ni-Ti powder is added in crucible, after sealing, continues to mix on ball mill
Expect 4h；Finally, binder is added in crucible, after sealing, all raw materials batch mixing 8h again completes tape casting suspension slurry
Preparation, the viscosity of the suspension slurry after preparation is 1.5Pa.S；
(4) suspension slurry is poured on surface to plate in the base vinyl film of silicon, scraper height is adjusted to 200 μm, along same
Slurry is equably cast on a carrier film by one direction；
(5) carrier film after curtain coating is placed in vacuum environment, vacuum degree is less than 1Pa, and drying temperature is 60 DEG C, dry
Time is 8h, between thickness is 140~150 μm after the casting films after drying are shunk.
Composite soldering film after drying is integrally removed from carrier silicon fiml, composite soldering film flexibility is very good, can be with
It arbitrarily folds and cuts, in Fig. 5 shown in (a).TiC even particulate dispersions are golden in binary Ni-Ti in composite soldering film after drying
Belong in powder, in microstructure such as attached drawing 5 shown in (b).It can implement to be brazed after composite soldering film is cut.Using above-mentioned multiple
125 ± 27MPa can be reached by closing the four-point bending intensity of solder film connection silicon carbide ceramics.
Claims (8)
1. a kind of preparation method of the ceramic granule reinforced composite material film of low content of organics, which is characterized in that including：
（1）Ceramic powder, metal-powder, dispersant and binder are uniformly dispersed in a solvent, suspension slurry is obtained after ball milling
Expect, the percent by volume of the ceramic powder and metal-powder is（10%~30%）：（70%~90%）, the dispersant and bonding
The gross mass of agent is no more than the 6wt.% of ceramic powder, metal-powder and solvent gross mass, wherein the dispersant is castor oil
Phosphate or/and castor oil, addition are 2~3wt.% of ceramic powder, metal-powder and solvent gross mass, the bonding
Agent is polyvinyl butyral, and addition is 2~3wt.% of ceramic powder, metal-powder and solvent gross mass, the metal
Powder be in Ag, Cu, Ti, Ni, Pd, In at least two or be at least containing two kinds of elements in Ag, Cu, Ti, Ni, Pd, In
Alloy powder, the ceramic powder are SiC, B4C 、TiC 、Si3N4Or TiB2；
（2）By the suspension slurry of gained according to required thickness tape casting at dry after composite soldering film, obtain described low having
The ceramic granule reinforced composite material film of machine object content.
2. preparation method according to claim 1, which is characterized in that step（1）Including：Ceramic powder, dispersant is molten
In solvent, then metal-powder, ball milling 2~6 hours is added in ball milling 8~16 hours；Finally add binder, ball milling 4~12
Hour, prepare the suspension slurry for tape casting.
3. preparation method according to claim 1, which is characterized in that the solid content of the suspension slurry is 22~30
vol.%。
4. preparation method according to claim 1, which is characterized in that the solvent is 2- butanone or/and ethyl alcohol.
5. preparation method according to claim 4, which is characterized in that the solvent is molten for the mixing of 2- butanone and ethyl alcohol
Liquid, the wherein mass ratio of 2- butanone and ethyl alcohol are（60~70）:（30~40）.
6. preparation method according to claim 1, which is characterized in that the average grain diameter of the ceramic powder is 5~20 μm,
The average grain diameter of the metal-powder is 1~50 μm.
7. preparation method according to claim 1, which is characterized in that the height of scraper is 50~200 μm in tape casting.
8. preparation method according to claim 1, which is characterized in that the environment of the drying is that vacuum degree is less than 1Pa, is done
Dry temperature is 50~60 DEG C, and drying time is 5~10 hours.
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| CN111153713A (en) * | 2020-01-15 | 2020-05-15 | 秦皇岛本征晶体科技有限公司 | Ceramic metallization slurry and preparation method and application thereof |
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| US20040124231A1 (en) * | 1999-06-29 | 2004-07-01 | Hasz Wayne Charles | Method for coating a substrate |
| ES2558877T3 (en) * | 2006-06-22 | 2016-02-09 | H.C. Starck Hermsdorf Gmbh | Procedure for the manufacture of molded bodies of refractory metal |
| CN101289328B (en) * | 2008-05-20 | 2011-01-19 | 西安理工大学 | Method for preparing metal-ceramic composite material |
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