CN101817684B - Method for coating h-BN coating on surface of porous Si3N4 substrate - Google Patents
Method for coating h-BN coating on surface of porous Si3N4 substrate Download PDFInfo
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- CN101817684B CN101817684B CN2010101324828A CN201010132482A CN101817684B CN 101817684 B CN101817684 B CN 101817684B CN 2010101324828 A CN2010101324828 A CN 2010101324828A CN 201010132482 A CN201010132482 A CN 201010132482A CN 101817684 B CN101817684 B CN 101817684B
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Abstract
The invention discloses a method for coating an h-BN coating on the surface of a porous Si3N4 substrate, which comprises the following steps of: 1, mixing Si3N4, Y2O3, Al2O3 and refinery coke in a mass ratio and grinding the mixture to prepare slurry; 2, drying and screening the slurry, pressing obtained powder into green compact and sintering the green compact in an N2 atmosphere to obtain the Si3N4 substrate; 3, washing and drying the Si3N4 substrate and coating H3BO3 onto the surface of the Si3N4 substrate; 4, heating the Si3N4 substrate coated with the H3BO3 and obtaining uniform B2O3 on the surface of the Si3N4 substrate; and 5, heating the Si3N4 substrate of which the surface has the B2O3 obtained in the step 4, and performing carbothermic reduction reaction to obtain the h-BN coating coated on the surface of the Si3N4 substrate. The method has the characteristics of low cost and simple operation; and a complex prepared structure integrates the advantages of two ceramic materials and can be widely applied to metal forming moulds.
Description
Technical field
The present invention relates to the method for porous matrix coating, particularly a kind of porous Si
3N
4Matrix surface covers the method that is coated with the h-BN coating.
Background technology
Porous Si
3N
4Pottery has good thermostability, corrosion resistance nature, antioxidant property and very high advantages such as physical strength as the structured material that high temperature uses down, aspect practical applications, demonstrates great potential and advantage.H-BN has the heat conductivility height, chemical property is stablized, almost all molten metals all is unreactiveness, resistance of oxidation is strong, thermostability is high and has performances such as very strong neutron receptivity and excellent electric insulating, so it has the high using value of potential in fields such as ceramic, fire-resistant, electrician, catalysis.The h-BN stupalith have very high thermal conductivity, excellent electric insulation performance, extremely low thermal expansivity and and the advantages such as not wellability of most metal, these character of himself have determined h-BN having rare advantage as advanced ceramic materials.But at present h-BN is relatively poor in ceramic mechanical property, also is not very extensive as the application of main components, does not have suitable method to come the h-BN of forms such as the particle of synthesis of nano yardstick, fiber and film in addition.In addition, because character such as the high-temperature stability of h-BN and low-down frictional coefficient make it in the high-temperature solid lubrication field, obtain using widely.As the h-BN of solid high temperature lubricant, it has higher heatproof characteristic and anti-portative power than some other lubricant, in corrosive atmosphere, also has advantages of higher stability, and nontoxic, look white, pollution-free etc. to environment and processed device.
Mostly that adopts at present the high-temperature chemical reaction preparation is the h-BN powder, as 1) inorganics and NH such as boron oxide compound, boron sodium salt
3Or N
2React; 2) borax, urea, two arteries and veins that contract, flesh, ammonia eyeball, Dyhard RU 100, sulphur arteries and veins or trimeric cyanamide etc. and NH
3Reaction; 3) boron simple substance and N
2Reaction etc.And high-quality h-BN coating adopts the vapour deposition process preparation more; These methods comprise chemical Vapor deposition process (CVD), Metalorganic Chemical Vapor Deposition (MOCVD), Low Pressure Chemical Vapor Deposition (LPCVD), ion assistance vapour deposition process (CVD of team), laser assistance vapour deposition process (LACVD) etc.; But the shortcoming of these methods is to cost an arm and a leg, complex process.
Summary of the invention
In order to overcome the defective of above-mentioned prior art, the object of the present invention is to provide a kind of porous Si
3N
4Matrix surface covers the method that is coated with the h-BN coating, utilizes the normal pressure-sintered porous silicon nitride ceramic sample of preparing, and guarantees the safety of matrix strength, utilizes H
3BO
3Decompose preparation B
2O
3Coating finally utilizes carbothermic reduction reaction with B
2O
3Coating changes the BN coating into, has guaranteed technologic stability, has low, the simple to operate characteristics of cost, and the composite structure of preparation combines the advantage of two kinds of stupaliths, can aspect metal molding die, be used widely.
In order to achieve the above object, technical scheme of the present invention is achieved in that
A kind of porous Si
3N
4Matrix surface covers the method that is coated with the h-BN coating, may further comprise the steps:
One, presses the Si of mass ratio with 30-50%
3N
4, 5%-7% Y
2O
3, 2%-6%A1
2O
3Mixing the ball grinder of packing into the refinery coke of 40-60%, is ball-milling medium with the absolute ethyl alcohol, with silicon nitride abrading-ball ball milling 24-48h, makes slip;
Two, with the slip that makes in 40-60 ℃ of loft drier dry 6-12 hour, cross 200 mesh sieves, obtain powder, the powder that obtains is pressed into the disk green compact, at N
21600 ℃ of-1800 ℃ of following sintering 2-3h in the atmosphere, N
2Pressure is 2-3 normal atmosphere, and obtaining void content is the Si of 25%-35%
3N
4Matrix;
Three, with the Si that sinters
3N
4Matrix is clean with surface cleaning with absolute ethyl alcohol, puts into drying baker 40-60 ℃ dry for standby then, again with the H of commercialization
3BO
3Evenly cover and be coated in Si
3N
4Matrix surface, required H
3BO
3Quality and Si
3N
4Surface of the base body is than being 0.2-0.6g/cm
2
Four, will cover and scribble H
3BO
3Si
3N
4Matrix is put into stove and is heated, and with the matrix 7-10 degree that tilts, Heating temperature is 500-700 ℃ during heating, and heating rate is 4-6 ℃/min, according to chemical equation 2H
3BO
3(S)=B
2O
3(s)+3H
2O (g) is at Si
3N
4Matrix surface obtains uniform B
2O
3
Five, surface in the step 4 had B
2O
3Si
3N
4Matrix is 4 atmospheric N at pressure
2Heat in the atmosphere, temperature is 1500 ℃-1700 ℃, utilizes carbothermic reduction reaction B
2O
3(s)+N
2(g)+and 3C (s) → 2BN (s)+3CO (g), form the h-BN coating, i.e. porous Si
3N
4Matrix surface covers and scribbles the h-BN coating.
The present invention utilizes porous Si
3N
4High temperature resistant, the pyrochemistry inertia that pottery and h-BN have reaches the not infiltrating characteristics with most metal, adopts simple carbon heat reducing to be reflected at porous Si
3N
4Matrix surface prepares the h-BN coating; It is being applied aspect accurate frock clamp of using in the glass-encapsulated of the smelting of non-ferrous metal and processing, glass melting and electron trade; For example this composite structure can be used as semi-conductor chip and outlet line welds, the ceramic welding mould of encapsulation usefulness; Be applicable to 600-950 ℃ of high-temperature soldering, encapsulation, and have high temperature medium-term and long-term use indeformable, the characteristics of sticking glass in the glass bulb encapsulation process; This composite structure also can be used as high technology ceramics mould and the frock clamp that the metallurgy of aluminium is used simultaneously, have aluminium liquid nonwetting, the characteristics of the long-term corrosion of anti-the aluminium alloy melt.The present invention has that cost is low, the measured characteristics of matter.
Description of drawings
Fig. 1 is embodiment 3B
2O
3Coating XRD figure spectrum.
Fig. 2 is that embodiment 3 carbothermic reduction temperature are the BN coating XRD figure spectrum under 1650 ℃.
Fig. 3 is that embodiment 3 carbothermic reduction temperature are the BN coating section SEM figure under 1650 ℃.
Fig. 4 is that embodiment 3 carbothermic reduction temperature are the BN coatingsurface SEM figure under 1650 ℃.
Embodiment
Embodiment one
Present embodiment may further comprise the steps:
One, presses mass ratio with 30% Si
3N
4, 5% Y
2O
3, 5%Al
2O
3Mixing the ball grinder of packing into 60% refinery coke, is ball-milling medium with the absolute ethyl alcohol, with silicon nitride abrading-ball ball milling 24h, makes slip;
Two, with the slip that makes in 40 ℃ of loft drier dry 12 hours, cross 200 mesh sieves, obtain powder, the powder that obtains is pressed into the disk green compact, at N
21600 ℃ of following sintering 2h in the atmosphere, N
2Pressure is 3 normal atmosphere, and the acquisition void content is 35% Si
3N
4Matrix;
Three, with the Si that sinters
3N
4Matrix is clean with surface cleaning with absolute ethyl alcohol, puts into 40 ℃ of dry for standby of drying baker then, again with the H of commercialization
3BO
3Evenly cover and be coated in Si
3N
4Matrix surface, required H
3BO
3Quality and Si
3N
4Surface of the base body is than being 0.2g/cm
2
Four, will cover and scribble H
3BO
3Si
3N
4Matrix is put into stove and is heated, and with matrix inclination 10 degree, Heating temperature is 700 ℃ during heating, and heating rate is 6 ℃/min, according to chemical equation 2H
3BO
3(S)=B
2O
3(s)+3H
2O (g) is at Si
3N
4Matrix surface obtains uniform B
2O
3
Five, surface in the step 4 had B
2O
3Si
3N
4Matrix is 4 atmospheric N at pressure
2Heat in the atmosphere, temperature is 1700 ℃, utilizes carbothermic reduction reaction B
2O
3(s)+N
2(g)+and 3C (s) → 2BN (s)+3CO (g), form the h-BN coating, i.e. porous Si
3N
4Matrix surface covers and scribbles the h-BN coating.
Embodiment two
Present embodiment may further comprise the steps:
One, presses mass ratio with 50% Si
3N
4, 4% Y
2O
3, 6%Al
2O
3Mixing the ball grinder of packing into 40% refinery coke, is ball-milling medium with the absolute ethyl alcohol, with silicon nitride abrading-ball ball milling 48h, makes slip;
Two, with the slip that makes in 60 ℃ of loft drier dry 6 hours, cross 200 mesh sieves, obtain powder, the powder that obtains is pressed into the disk green compact, at N
21800 ℃ of following sintering 2.8h in the atmosphere, N
2Pressure is 2 normal atmosphere, and the acquisition void content is 25% Si
3N
4Matrix;
Three, with the Si that sinters
3N
4Matrix is clean with surface cleaning with absolute ethyl alcohol, puts into 60 ℃ of dry for standby of drying baker then, again with the H of commercialization
3BO
3Evenly cover and be coated in Si
3N
4Matrix surface, required H
3BO
3Quality and Si
3N
4Surface of the base body is than being 0.3g/cm
2
Four, will cover and scribble H
3BO
3Si
3N
4Matrix is put into stove and is heated, and with matrix inclination 8 degree, Heating temperature is 500 ℃ during heating, and heating rate is 5 ℃/min, according to chemical equation 2H
3BO
3(S)=B
2O
3(s)+3H
2O (g) is at Si
3N
4Matrix surface obtains uniform B
2O
3
Five, surface in the step 4 had B
2O
3Si
3N
4Matrix is 4 atmospheric N at pressure
2Heat in the atmosphere, temperature is 1600 ℃, utilizes carbothermic reduction reaction B
2O
3(s)+N
2(g)+and 3C (s) → 2BN (s)+3CO (g), form the h-BN coating, i.e. porous Si
3N
4Matrix surface covers and scribbles the h-BN coating.
Embodiment three
Present embodiment may further comprise the steps:
One, presses mass ratio with 41% Si
3N
4, 5% Y
2O
3, 4%Al
2O
3Mixing the ball grinder of packing into 50% refinery coke, is ball-milling medium with the absolute ethyl alcohol, with silicon nitride abrading-ball ball milling 24h, makes slip;
Two, with the slip that makes in 50 ℃ of loft drier dry 9 hours, cross 200 mesh sieves, obtain powder, the powder that obtains is pressed into the disk green compact, at N
21650 ℃ of following sintering 3h in the atmosphere, N
2Pressure is 2 normal atmosphere, and the acquisition void content is 28% Si
3N
4Matrix;
Three, with the Si that sinters
3N
4Matrix is clean with surface cleaning with absolute ethyl alcohol, puts into 50 ℃ of dry for standby of drying baker then, again with the H of commercialization
3BO
3Evenly cover and be coated in Si
3N
4Matrix surface, required H
3BO
3Quality and Si
3N
4Surface of the base body is than being 0.6g/cm
2
Four, will cover and scribble H
3BO
3Si
3N
4Matrix is put into stove and is heated, and with matrix inclination 10 degree, Heating temperature is 600 ℃ during heating, and heating rate is 6 ℃/min, according to chemical equation 2H
3BO
3(S)=B
2O
3(s)+3H
2O (g) is at Si
3N
4Matrix surface obtains uniform B
2O
3
Five, surface in the step 4 had B
2O
3Si
3N
4Matrix is 4 atmospheric N at pressure
2Heat in the atmosphere, temperature is 1650 ℃, utilizes carbothermic reduction reaction B
2O
3(s)+N
2(g)+and 3C (s) → 2BN (s)+3CO (g), form the h-BN coating, i.e. porous Si
3N
4Matrix surface covers and scribbles the h-BN coating.
Fig. 1 is B in the present embodiment
2O
3Coating XRD figure spectrum, as can be seen from Figure 1, through preceding four steps of present embodiment, at Si
3N
4Matrix surface obtains B
2O
3Coating.
Fig. 2 is that the carbothermic reduction temperature is the coating XRD figure spectrum under 1650 ℃ in the present embodiment, as can be seen from Figure 2, through present embodiment at Si
3N
4Matrix surface obtains the h-BN coating, and Beta-Si is arranged
3N
4Appearance be because coating is thinner, X ray squeezes into that matrix causes.
Fig. 3 is that the carbothermic reduction temperature is the coating section SEM figure under 1650 ℃ in the present embodiment.As can be seen from Figure 3, the BN coat-thickness is approximately 1.6 μ m, the inner no significant defect of coating, and coating and matrix bond are better.
Fig. 4 is that the carbothermic reduction temperature is the BN coatingsurface SEM figure under 1650 ℃ in the present embodiment.As can beappreciated from fig. 4, BN coatingsurface opposed flattened, but have pit to occur, analyzing reason is because B
2O
3Vaporization at high temperature due to.
Embodiment four
Present embodiment may further comprise the steps:
One, presses mass ratio with 35% Si
3N
4, 7% Y
2O
3, 2%Al
2O
3Mixing the ball grinder of packing into 56% refinery coke, is ball-milling medium with the absolute ethyl alcohol, with silicon nitride abrading-ball ball milling 36h, makes slip;
Two, with the slip that makes in 45 ℃ of loft drier dry 10 hours, cross 200 mesh sieves, obtain powder, the powder that obtains is pressed into the disk green compact, at N
21700 ℃ of following sintering 2.5h in the atmosphere, N
2Pressure is 3 normal atmosphere, and the acquisition void content is 30% Si
3N
4Matrix;
Three, with the Si that sinters
3N
4Matrix is clean with surface cleaning with absolute ethyl alcohol, puts into 55 ℃ of dry for standby of drying baker then, again with the H of commercialization
3BO
3Evenly cover and be coated in Si
3N
4Matrix surface, required H
3BO
3Quality and Si
3N
4Surface of the base body is than being 0.4g/cm
2
Four, will cover and scribble H
3BO
3Si
3N
4Matrix is put into stove and is heated, and with matrix inclination 7 degree, Heating temperature is 650 ℃ during heating, and heating rate is 4 ℃/min, according to chemical equation 2H
3BO
3(S)=B
2O
3(s)+3H
2O (g) is at Si
3N
4Matrix surface obtains uniform B
2O
3
Five, surface in the step 4 had B
2O
3Si
3N
4Matrix is 4 atmospheric N at pressure
2Heat in the atmosphere, temperature is 1600 ℃, utilizes carbothermic reduction reaction B
2O
3(s)+N
2(g)+and 3C (s) → 2BN (s)+3CO (g), form the h-BN coating, i.e. porous Si
3N
4Matrix surface covers and scribbles the h-BN coating.
Embodiment five
Present embodiment may further comprise the steps:
One, presses mass ratio with 46% Si
3N
4, 6% Y
2O
3, 3%Al
2O
3Mixing the ball grinder of packing into 45% refinery coke, is ball-milling medium with the absolute ethyl alcohol, with silicon nitride abrading-ball ball milling 40h, makes slip;
Two, with the slip that makes in 55 ℃ of loft drier dry 8 hours, cross 200 mesh sieves, obtain powder, the powder that obtains is pressed into the disk green compact, at N
21750 ℃ of following sintering 2.2h in the atmosphere, N
2Pressure is 2.5 normal atmosphere, and the acquisition void content is 26% Si
3N
4Matrix;
Three, with the Si that sinters
3N
4Matrix is clean with surface cleaning with absolute ethyl alcohol, puts into 45 ℃ of dry for standby of drying baker then, again with the H of commercialization
3BO
3Evenly cover and be coated in Si
3N
4Matrix surface, required H
3BO
3Quality and Si
3N
4Surface of the base body is than being 0.5g/cm
2
Four, will cover and scribble H
3BO
3Si
3N
4Matrix is put into stove and is heated, and with matrix inclination 9 degree, Heating temperature is 550 ℃ during heating, and heating rate is 5.5 ℃/min, according to chemical equation 2H
3BO
3(S)=B
2O
3(s)+3H
2O (g) is at Si
3N
4Matrix surface obtains uniform B
2O
3
Five, surface in the step 4 had B
2O
3Si
3N
4Matrix is 4 atmospheric N at pressure
2Heat in the atmosphere, temperature is 1580 ℃, utilizes carbothermic reduction reaction B
2O
3(s)+N
2(g)+and 3C (s) → 2BN (s)+3CO (g), form the h-BN coating, i.e. porous Si
3N
4Matrix surface covers and scribbles the h-BN coating.
Claims (6)
1. porous Si
3N
4Matrix surface covers the method that is coated with the h-BN coating, it is characterized in that, may further comprise the steps:
One, presses the Si of mass ratio with 30-50%
3N
4, 5%-7% Y
2O
3, 2%-6%Al
2O
3Mixing the ball grinder of packing into the refinery coke of 40-60%, is ball-milling medium with the absolute ethyl alcohol, with silicon nitride abrading-ball ball milling 24-48h, makes slip;
Two, with the slip that makes in 40-60 ℃ of loft drier dry 6-12 hour, cross 200 mesh sieves, obtain powder, the powder that obtains is pressed into the disk green compact, at N
21600 ℃ of-1800 ℃ of following sintering 2-3h in the atmosphere, N
2Pressure is 2-3 normal atmosphere, and obtaining void content is the Si of 25%-35%
3N
4Matrix;
Three, with the Si that sinters
3N
4Matrix is clean with surface cleaning with absolute ethyl alcohol, puts into drying baker 40-60 ℃ dry for standby then, again with the H of commercialization
3BO
3Evenly cover and be coated in Si
3N
4Matrix surface, required H
3BO
3Quality and Si
3N
4Surface of the base body is than being 0.2-0.6g/cm
2
Four, will cover and scribble H
3BO
3Si
3N
4Matrix is put into stove and is heated, and with the matrix 7-10 degree that tilts, Heating temperature is 500-700 ℃ during heating, and heating rate is 4-6 ℃/min, according to chemical equation 2H
3BO
3(S)=B
2O
3(s)+3H
2O (g) is at Si
3N
4Matrix surface obtains uniform B
2O
3
Five, surface in the step 4 had B
2O
3Si
3N
4Matrix is 4 atmospheric N at pressure
2Heat in the atmosphere, temperature is 1500 ℃-1700 ℃, utilizes carbothermic reduction reaction B
2O
3(s)+N
2(g)+and 3C (s) → 2BN (s)+3CO (g), form the h-BN coating, i.e. porous Si
3N
4Matrix surface covers and scribbles the h-BN coating.
2. a kind of porous Si according to claim 1
3N
4Matrix surface covers the method that is coated with the h-BN coating, it is characterized in that, may further comprise the steps:
One, presses mass ratio with 30% Si
3N
4, 5% Y
2O
3, 5%Al
2O
3Mixing the ball grinder of packing into 60% refinery coke, is ball-milling medium with the absolute ethyl alcohol, with silicon nitride abrading-ball ball milling 24h, makes slip;
Two, with the slip that makes in 40 ℃ of loft drier dry 12 hours, cross 200 mesh sieves, obtain powder, the powder that obtains is pressed into the disk green compact, at N
21600 ℃ of following sintering 2h in the atmosphere, N
2Pressure is 3 normal atmosphere, and the acquisition void content is 35% Si
3N
4Matrix;
Three, with the Si that sinters
3N
4Matrix is clean with surface cleaning with absolute ethyl alcohol, puts into 40 ℃ of dry for standby of drying baker then, again with the H of commercialization
3BO
3Evenly cover and be coated in Si
3N
4Matrix surface, required H
3BO
3Quality and Si
3N
4Surface of the base body is than being 0.2g/cm
2
Four, will cover and scribble H
3BO
3Si
3N
4Matrix is put into stove and is heated, and with matrix inclination 10 degree, Heating temperature is 700 ℃ during heating, and heating rate is 6 ℃/min, according to chemical equation 2H
3BO
3(S)=B
2O
3(s)+3H
2O (g) is at Si
3N
4Matrix surface obtains uniform B
2O
3
Five, surface in the step 4 had B
2O
3Si
3N
4Matrix is 4 atmospheric N at pressure
2Heat in the atmosphere, temperature is 1700 ℃, utilizes carbothermic reduction reaction B
2O
3(s)+N
2(g)+and 3C (s) → 2BN (s)+3CO (g), form the h-BN coating, i.e. porous Si
3N
4Matrix surface covers and scribbles the h-BN coating.
3. a kind of porous Si according to claim 1
3N
4Matrix surface covers the method that is coated with the h-BN coating, it is characterized in that, may further comprise the steps:
One, presses mass ratio with 41% Si
3N
4, 5% Y
2O
3, 4%Al
2O
3Mixing the ball grinder of packing into 50% refinery coke, is ball-milling medium with the absolute ethyl alcohol, with silicon nitride abrading-ball ball milling 24h, makes slip;
Two, with the slip that makes in 50 ℃ of loft drier dry 9 hours, cross 200 mesh sieves, obtain powder, the powder that obtains is pressed into the disk green compact, at N
21650 ℃ of following sintering 3h in the atmosphere, N
2Pressure is 2 normal atmosphere, and the acquisition void content is 28% Si
3N
4Matrix;
Three, with the Si that sinters
3N
4Matrix is clean with surface cleaning with absolute ethyl alcohol, puts into 50 ℃ of dry for standby of drying baker then, again with the H of commercialization
3BO
3Evenly cover and be coated in Si
3N
4Matrix surface, required H
3BO
3Quality and Si
3N
4Surface of the base body is than being 0.6g/cm
2
Four, will cover and scribble H
3BO
3Si
3N
4Matrix is put into stove and is heated, and with matrix inclination 10 degree, Heating temperature is 600 ℃ during heating, and heating rate is 6 ℃/min, according to chemical equation 2H
3BO
3(S)=B
2O
3(s)+3H
2O (g) is at Si
3N
4Matrix surface obtains uniform B
2O
3
Five, surface in the step 4 had B
2O
3Si
3N
4Matrix is 4 atmospheric N at pressure
2Heat in the atmosphere, temperature is 1650 ℃, utilizes carbothermic reduction reaction B
2O
3(s)+N
2(g)+and 3C (s) → 2BN (s)+3CO (g), form the h-BN coating, i.e. porous Si
3N
4Matrix surface covers and scribbles the h-BN coating.
4. a kind of porous Si according to claim 1
3N
4Matrix surface covers the method that is coated with the h-BN coating, it is characterized in that, may further comprise the steps:
One, presses mass ratio with 35% Si
3N
4, 7% Y
2O
3, 2%Al
2O
3Mixing the ball grinder of packing into 56% refinery coke, is ball-milling medium with the absolute ethyl alcohol, with silicon nitride abrading-ball ball milling 36h, makes slip;
Two, with the slip that makes in 45 ℃ of loft drier dry 10 hours, cross 200 mesh sieves, obtain powder, the powder that obtains is pressed into the disk green compact, at N
21700 ℃ of following sintering 2.5h in the atmosphere, N
2Pressure is 3 normal atmosphere, and the acquisition void content is 30% Si
3N
4Matrix;
Three, with the Si that sinters
3N
4Matrix is clean with surface cleaning with absolute ethyl alcohol, puts into 55 ℃ of dry for standby of drying baker then, again with the H of commercialization
3BO
3Evenly cover and be coated in Si
3N
4Matrix surface, required H
3BO
3Quality and Si
3N
4Surface of the base body is than being 0.4g/cm
2
Four, will cover and scribble H
3BO
3Si
3N
4Matrix is put into stove and is heated, and with matrix inclination 7 degree, Heating temperature is 650 ℃ during heating, and heating rate is 4 ℃/min, according to chemical equation 2H
3BO
3(S)=B
2O
3(s)+3H
2O (g) is at Si
3N
4Matrix surface obtains uniform B
2O
3
Five, surface in the step 4 had B
2O
3Si
3N
4Matrix is 4 atmospheric N at pressure
2Heat in the atmosphere, temperature is 1600 ℃, utilizes carbothermic reduction reaction B
2O
3(s)+N
2(g)+and 3C (s) → 2BN (s)+3CO (g), form the h-BN coating, i.e. porous Si
3N
4Matrix surface covers and scribbles the h-BN coating.
5. a kind of porous Si according to claim 1
3N
4Matrix surface covers the method that is coated with the h-BN coating, it is characterized in that, may further comprise the steps:
One, presses mass ratio with 46% Si
3N
4, 6% Y
2O
3, 3%Al
2O
3Mixing the ball grinder of packing into 45% refinery coke, is ball-milling medium with the absolute ethyl alcohol, with silicon nitride abrading-ball ball milling 40h, makes slip;
Two, with the slip that makes in 55 ℃ of loft drier dry 8 hours, cross 200 mesh sieves, obtain powder, the powder that obtains is pressed into the disk green compact, at N
21750 ℃ of following sintering 2.2h in the atmosphere, N
2Pressure is 2.5 normal atmosphere, and the acquisition void content is 26% Si
3N
4Matrix;
Three, with the Si that sinters
3N
4Matrix is clean with surface cleaning with absolute ethyl alcohol, puts into 45 ℃ of dry for standby of drying baker then, again with the H of commercialization
3BO
3Evenly cover and be coated in Si
3N
4Matrix surface, required H
3BO
3Quality and Si
3N
4Surface of the base body is than being 0.5g/cm
2
Four, will cover and scribble H
3BO
3Si
3N
4Matrix is put into stove and is heated, and with matrix inclination 9 degree, Heating temperature is 550 ℃ during heating, and heating rate is 5.5 ℃/min, according to chemical equation 2H
3BO
3(S)=B
2O
3(s)+3H
2O (g) is at Si
3N
4Matrix surface obtains uniform B
2O
3
Five, surface in the step 4 had B
2O
3Si
3N
4Matrix is 4 atmospheric N at pressure
2Heat in the atmosphere, temperature is 1580 ℃, utilizes carbothermic reduction reaction B
2O
3(s)+N
2(g)+and 3C (s) → 2BN (s)+3CO (g), form the h-BN coating, i.e. porous Si
3N
4Matrix surface covers and scribbles the h-BN coating.
6. porous Si
3N
4Matrix surface covers the method that is coated with the h-BN coating, it is characterized in that, may further comprise the steps:
One, presses mass ratio with 50% Si
3N
4, 4% Y
2O
3, 6%Al
2O
3Mixing the ball grinder of packing into 40% refinery coke, is ball-milling medium with the absolute ethyl alcohol, with silicon nitride abrading-ball ball milling 48h, makes slip;
Two, with the slip that makes in 60 ℃ of loft drier dry 6 hours, cross 200 mesh sieves, obtain powder, the powder that obtains is pressed into the disk green compact, at N
21800 ℃ of following sintering 2.8h in the atmosphere, N
2Pressure is 2 normal atmosphere, and the acquisition void content is 25% Si
3N
4Matrix;
Three, with the Si that sinters
3N
4Matrix is clean with surface cleaning with absolute ethyl alcohol, puts into 60 ℃ of dry for standby of drying baker then, again with the H of commercialization
3BO
3Evenly cover and be coated in Si
3N
4Matrix surface, required H
3BO
3Quality and Si
3N
4Surface of the base body is than being 0.3g/cm
2
Four, will cover and scribble H
3BO
3Si
3N
4Matrix is put into stove and is heated, and with matrix inclination 8 degree, Heating temperature is 500 ℃ during heating, and heating rate is 5 ℃/min, according to chemical equation 2H
3BO
3(S)=B
2O
3(s)+3H
2O (g) is at Si
3N
4Matrix surface obtains uniform B
2O
3
Five, surface in the step 4 had B
2O
3Si
3N
4Matrix is 4 atmospheric N at pressure
2Heat in the atmosphere, temperature is 1600 ℃, utilizes carbothermic reduction reaction B
2O
3(s)+N
2(g)+and 3C (s) → 2BN (s)+3CO (g), form the h-BN coating, i.e. porous Si
3N
4Matrix surface covers and scribbles the h-BN coating.
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CN102660261B (en) * | 2012-04-19 | 2014-10-22 | 中国科学技术大学 | Preparation method of silicon oxynitride fluorescent powder |
CN103708843A (en) * | 2013-12-20 | 2014-04-09 | 中钢集团洛阳耐火材料研究院有限公司 | Boron nitride coating and application method |
US9732005B2 (en) * | 2014-04-07 | 2017-08-15 | United Technologies Corporation | Method of forming in-situ boron nitride for ceramic matrix composite environmental protection |
EP4131339A3 (en) * | 2016-05-12 | 2023-02-15 | GlobalWafers Co., Ltd. | Direct formation of hexagonal boron nitride on silicon based dielectrics |
CN108046808B (en) * | 2018-01-05 | 2020-08-11 | 广东工业大学 | Si3N4Gradient material and preparation method thereof |
CN108455540A (en) * | 2018-03-14 | 2018-08-28 | 宁夏艾森达新材料科技有限公司 | The processing method of aluminium nitride ceramics sintering boron nitride stove |
CN108395286B (en) * | 2018-03-14 | 2021-02-05 | 宁夏艾森达新材料科技有限公司 | Method for efficiently removing oxygen impurities in boron nitride furnace for sintering aluminum nitride ceramics |
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Title |
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Yongfeng Li et al..Interface structure and formation mechanism of BN/intergranular amorphous phase in pressureless sintered Si3N4/BN composites.《Scripta Materialia》.2010,第63卷185-188. * |
王向东 等.可加工Si3N4/BN复相陶瓷的制备及性能研究.《稀有金属材料与工程》.2003,第32卷(第7期),498-501. * |
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