CN110483091A - A kind of connection method of porous silicon nitride ceramic - Google Patents
A kind of connection method of porous silicon nitride ceramic Download PDFInfo
- Publication number
- CN110483091A CN110483091A CN201910908744.6A CN201910908744A CN110483091A CN 110483091 A CN110483091 A CN 110483091A CN 201910908744 A CN201910908744 A CN 201910908744A CN 110483091 A CN110483091 A CN 110483091A
- Authority
- CN
- China
- Prior art keywords
- porous silicon
- nitride
- silicon substrate
- articulamentum
- connection method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/001—Joining burned ceramic articles with other burned ceramic articles or other articles by heating directly with other burned ceramic articles
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/04—Ceramic interlayers
- C04B2237/08—Non-oxidic interlayers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/32—Ceramic
- C04B2237/36—Non-oxidic
- C04B2237/368—Silicon nitride
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/52—Pre-treatment of the joining surfaces, e.g. cleaning, machining
Abstract
The present invention relates to silicon nitride ceramics sintering arts, it in particular is a kind of connection method of porous silicon nitride ceramic, including nitride porous silicon substrate I, articulamentum and nitride porous silicon substrate II, nitride porous silicon substrate I and nitride porous silicon substrate II are connected with each other by the articulamentum by sintering, articulamentum grows the nitride porous silicon substrate I and nitride porous silicon substrate II for depending on two sides, the nitride porous silicon substrate I and nitride porous silicon substrate II of the mutually interspersed bridge joint two sides of the articulamentum after growth;The sintering connection between porous silicon nitride ceramic may be implemented, the silicon nitride grain of articulamentum depends on two sides nitride porous silicon substrate I to be connected and nitride porous silicon substrate II is grown, and it is not based on articulamentum and individually grows, therefore articulamentum does not generate apparent contraction during the sintering process, solves the problems, such as that articulamentum cracks because sintering shrinkage is excessive.
Description
Technical field
The present invention relates to silicon nitride ceramics sintering arts, are in particular a kind of connection sides of porous silicon nitride ceramic
Method.
Background technique
Silicon nitride ceramics has high intensity, high tenacity, low thermal coefficient of expansion and good high-temperature stability, flies in ultrahigh speed
Row device antenna house field has broad application prospects.The major function of aerospace craft antenna house be carrying, heat-insulated, water conservancy diversion and thoroughly
Wave etc..The dielectric constant higher 7~8.5 of compact silicon nitride ceramics, is not able to satisfy the demand of antenna house wave transparent, it is therefore desirable to by nitrogen
SiClx ceramic porousization is to reduce its dielectric constant.The silicon nitride ceramics of the single porosity is difficult to realize carrying and heat-insulated simultaneously
Function, more feasible method are the porous silicon nitride ceramics for preparing the connection of high/low stomata, and low stomata layer is responsible for carrying and high
Stomata layer is responsible for heat-insulated.It prepares graded pore structure also and the thermal shock resistance of ceramic material can be improved, further increase antenna house
Reliability.In addition, the silicon nitride ceramics of the different porositys is connected by certain way, the wideband wave transparent of antenna house can also be achieved.
Due to the difference of two sides substrate pore rate, articulamentum can have biggish internal stress, easily open the junction of ceramics
It splits.Biggish contraction can also occur for the ceramic direct sintering of articulamentum, further increase the internal stress of linkage interface, biggish to answer
Power even can directly destroy the silicon nitride matrix of high stomata.
Summary of the invention
The object of the present invention is to provide a kind of connection methods of porous silicon nitride ceramic, can solve articulamentum because sintering is received
Contract it is excessive and the problem of crack.
The purpose of the present invention is achieved through the following technical solutions:
A kind of connection method of porous silicon nitride ceramic, including nitride porous silicon substrate I, articulamentum and nitride porous silicon substrate
Nitride porous silicon substrate I and nitride porous silicon substrate II are connected with each other by body II, the articulamentum by sintering, articulamentum growth
The nitride porous silicon substrate I and nitride porous silicon substrate II for depending on two sides, the mutually interspersed bridge joint two sides of articulamentum after growth
Nitride porous silicon substrate I and nitride porous silicon substrate II.
As advanced optimizing for the technical program, a kind of connection method of porous silicon nitride ceramic of the present invention, the company
It connects layer and is laminated by tri- layers of raw material of A-B-A and formed, wherein A layers of the articulamentum of two sides is made of ceramic powder A, and ceramic powder A is by α-
Si3N4It forms, is made wherein being located in the middle B layers of articulamentum of ceramic powder B, ceramic powder B is by α-Si with sintering aid3N4
Composition.
As advanced optimizing for the technical program, a kind of connection method of porous silicon nitride ceramic of the invention, described two
α-Si in side A layers3N4Mass ratio with sintering aid is 1:9~19.
As advanced optimizing for the technical program, a kind of connection method of porous silicon nitride ceramic of the present invention, the burning
Auxiliary agent is tied by Y2O3And Al2O3Powder composition, Y2O3And Al2O3Mass ratio be 1:0.6~0.8.
As advanced optimizing for the technical program, a kind of connection method of porous silicon nitride ceramic of the present invention, the company
The green compact for connecing layer are prepared by tape casting, and specific preparation process includes the following steps:
Step 1: deionized water, ceramic powder A and dispersing agent ball milling mixing are prepared into mixed slurry A;
Step 2: deionized water, ceramic powder B and dispersing agent ball milling mixing are prepared into mixed slurry B;
Step 3: it is separately added into binder, plasticizer in mixed slurry A and mixed slurry B, continuess to mix and respectively obtains stream
Prolong slurry A and casting slurry B;
Step 4: casting slurry A and casting slurry B after de-bubble, is poured on release film and is cast under vacuum conditions
Molding, the slurry after curtain coating is spontaneously dried at room temperature, is then removed from release film, respectively obtains A layers of articulamentum
Green compact and B layers of articulamentum of green compact.
As advanced optimizing for the technical program, a kind of connection method of porous silicon nitride ceramic of the present invention is described viscous
Tying agent is in polyvinyl alcohol or acrylic emulsion, and the mass ratio of ceramic powder and bonding agent is 1:0.004~0.008, plasticizer
For one or both of glycerol and polyethylene glycol, the mass ratio of ceramic powder and plasticizer is 1:0.008~0.016.
As advanced optimizing for the technical program, a kind of connection method of porous silicon nitride ceramic of the present invention is described more
The matrix surface of hole silicon nitride matrix I and nitride porous silicon substrate II is both needed to be polished with sand paper, after polishing be cleaned by ultrasonic and do
It is dry.
As advanced optimizing for the technical program, a kind of connection method of porous silicon nitride ceramic of the present invention is being sintered
By nitride porous silicon substrate I, articulamentum and nitride porous silicon substrate II according to along I-articulamentum of nitride porous silicon substrate-before connection
The sequence sequence of nitride porous silicon substrate II stacks and dumping in air.
As advanced optimizing for the technical program, a kind of connection method of porous silicon nitride ceramic of the present invention, the burning
Become gas pressure sintering, sintering temperature is 1700~1850 DEG C, and soaking time is 0.5~3 hour, and nitrogen pressure is 0.4~1MPa.
As advanced optimizing for the technical program, a kind of connection method of porous silicon nitride ceramic of the present invention, the burning
The pressure of 0.5~4MPa need to be applied when knot on nitride porous silicon substrate I and nitride porous silicon substrate II.
A kind of connection method of porous silicon nitride ceramic of the invention has the beneficial effect that
A kind of connection method of porous silicon nitride ceramic of the present invention, the sintering that may be implemented between porous silicon nitride ceramic connect
It connecing, the silicon nitride grain of articulamentum depends on two sides nitride porous silicon substrate I to be connected and nitride porous silicon substrate II is grown,
And be not based on articulamentum and individually grow, therefore articulamentum does not generate apparent contraction during the sintering process, efficiently solve connection
Layer because sintering shrinkage is excessive crack the problem of.
Detailed description of the invention
The present invention will be further described in detail with specific implementation method with reference to the accompanying drawing.
Fig. 1 is the SEM photograph schematic diagram of initial stage of sintering articulamentum of the invention;
Fig. 2 is the SEM spectrum schematic diagram of abundant sintered articulamentum of the invention.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Specific embodiment 1:
Illustrate present embodiment, a kind of connection method of porous silicon nitride ceramic, including nitride porous below with reference to Fig. 1-2
Silicon substrate I 1, articulamentum and nitride porous silicon substrate II 2, the articulamentum is by sintering by nitride porous silicon substrate I 1 and porous
Silicon nitride matrix II 2 is connected with each other, and articulamentum grows the nitride porous silicon substrate I 1 and nitride porous silicon substrate for depending on two sides
II 2, the nitride porous silicon substrate I 1 and nitride porous silicon substrate II 2 of the mutually interspersed bridge joint two sides of articulamentum after growth.
The articulamentum is laminated by tri- layers of raw material of A-B-A and is formed, and wherein A layers of the articulamentum of two sides is made of ceramic powder A,
Ceramic powder A is by α-Si3N4It forms, is made wherein being located in the middle B layers of articulamentum of ceramic powder B, ceramic powder with sintering aid
Body B is by α-Si3N4Composition.
α-Si in described two sides A layers3N4Mass ratio with sintering aid is 1:9~19.
The sintering aid is by Y2O3And Al2O3Powder composition, Y2O3And Al2O3Mass ratio be 1:0.6~0.8.
The green compact of the articulamentum are prepared by tape casting, and specific preparation process includes the following steps:
Step 1: deionized water, ceramic powder A and dispersing agent ball milling mixing are prepared into mixed slurry A;
Step 2: deionized water, ceramic powder B and dispersing agent ball milling mixing are prepared into mixed slurry B;
Step 3: it is separately added into binder, plasticizer in mixed slurry A and mixed slurry B, continuess to mix and respectively obtains stream
Prolong slurry A and casting slurry B;
Step 4: casting slurry A and casting slurry B after de-bubble, is poured on release film and is cast under vacuum conditions
Molding, the slurry after curtain coating is spontaneously dried at room temperature, is then removed from release film, respectively obtains A layers of articulamentum
Green compact and B layers of articulamentum of green compact.
The binder is in polyvinyl alcohol or acrylic emulsion, and the mass ratio of ceramic powder and bonding agent is 1:0.004
~0.008, plasticizer is one or both of glycerol and polyethylene glycol, and the mass ratio of ceramic powder and plasticizer is 1:
0.008~0.016.
The matrix surface of the nitride porous silicon substrate I 1 and nitride porous silicon substrate II 2 is both needed to be polished with sand paper, polishing
Afterwards with ultrasonic cleaning and drying.
By nitride porous silicon substrate I 1, articulamentum and nitride porous silicon substrate II 2 according to along porous nitrogen before sintering connection
I 1- articulamentum of SiClx matrix-nitride porous silicon substrate II 2 sequence sequence stacks and dumping in air.
Described to be sintered to gas pressure sintering, sintering temperature is 1700~1850 DEG C, and soaking time is 0.5~3 hour, nitrogen pressure
Power is 0.4~1MPa.
The pressure of 0.5~4MPa need to be applied when the sintering on nitride porous silicon substrate I 1 and nitride porous silicon substrate II 2
Power.
As seen from Figure 1, during the sintering process, growing up for the silicon nitride grain of articulamentum is to depend on two sides nitride porous
Silicon substrate I 1 and nitride porous silicon substrate II 2, and be not based on articulamentum itself, thus articulamentum do not occur during the sintering process it is bright
It is aobvious to shrink.If Fig. 2 can be seen that, it is sintered the later period, the silicon nitride grain of articulamentum is sufficiently grown up, mutually interspersed bridge joint, crystal grain ruler
It is very little similar to two sides nitride porous silicon substrate I 1 and nitride porous silicon substrate II 2 to draw ratio, therefore articulamentum has higher connection
Intensity.
Specific embodiment 2:
Illustrate that present embodiment, present embodiment are described further embodiment one below with reference to Fig. 1-2, Yi Zhongduo
The connection method of hole silicon nitride ceramics, comprising the following steps:
Step 1: by deionized water, ceramic powder A and dispersing agent ball milling mixing 12h, the volume of ceramic powder A in slurry
Score is 30~45%, and dispersing agent is one of polyacrylic acid and tetramethylammonium hydroxide, the matter of ceramic powder A and dispersing agent
Amount is than being 1:0.004~0.008, by deionized water, ceramic powder B and dispersing agent ball milling mixing 12h, ceramic powder B in slurry
Volume fraction be 30~45%, dispersing agent is one of polyacrylic acid and tetramethylammonium hydroxide, ceramic powder B and dispersion
The mass ratio of agent is 1:0.004~0.008, and ceramic powder A is by α-Si3N4It is formed with sintering aid, sintering aid and α-
Si3N4Mass ratio be 1:9~19, sintering aid is by Y2O3And Al2O3Powder composition, Y2O3And Al2O3Mass ratio be 1:
0.6~0.8, ceramic powder B are α-Si3N4;
Step 2: binder, plasticizer is added into mixed slurry A and mixed slurry B respectively, 30min is continuesd to mix, point
Casting slurry A and casting slurry B are not obtained, and binder is one of polyvinyl alcohol and acrylic emulsion, ceramic powder A or B
Mass ratio with bonding agent is 1:0.004~0.008, and plasticizer is one or both of glycerol and polyethylene glycol, ceramic powder
The mass ratio of body A or B and plasticizer is 1:0.008~0.016;
Step 3: being poured over release film for after casting slurry A and casting slurry B under vacuum conditions de-bubble 20min respectively
Upper carry out tape casting, molding scraper speed are 10cm/min, and edge height is 0.05~0.2mm, by the slurry after curtain coating
Natural drying 12h is carried out at room temperature, is then removed from release film, and A layers of articulamentum of green compact and B layers of articulamentum of life are obtained
Base;
Step 4: nitride porous silicon substrate I 1 and II 2 surface of nitride porous silicon substrate are polished with 800~1600 mesh sand paper,
Afterwards with ultrasonic cleaning and drying;
Step 5: by raw material in the way of I 1-A layers of-B layers of-A layers-nitride porous silicon substrate II 2 of nitride porous silicon substrate
It laminates and dumping, dump temperature is 600 DEG C in air, heating rate is 0.3~1 DEG C/min, and soaking time is 2~4 hours;
It is sintered Step 6: the raw material after laminating is placed in air pressure furnace, sintering temperature is 1700~1850 DEG C, soaking time
It is 0.5~3 hour, nitrogen pressure is 0.4~1MPa, when sintering, by nitride porous silicon substrate I 1 and nitride porous silicon substrate
Weight is placed on body II 2 to apply the pressure of 0.5~4MPa;
As seen from Figure 1, during the sintering process, growing up for the silicon nitride grain of articulamentum is to depend on two sides nitride porous
Silicon substrate I 1 and nitride porous silicon substrate II 2, and be not based on articulamentum itself, thus articulamentum do not occur during the sintering process it is bright
It is aobvious to shrink.If Fig. 2 can be seen that, it is sintered the later period, the silicon nitride grain of articulamentum is sufficiently grown up, mutually interspersed bridge joint, crystal grain ruler
It is very little similar to two sides nitride porous silicon substrate I 1 and nitride porous silicon substrate II 2 to draw ratio, therefore articulamentum has higher connection
Intensity.
Specific embodiment 3:
Illustrate that present embodiment, present embodiment are described further embodiment one below with reference to Fig. 1-2,
Step 1: by deionized water, ceramic powder A and dispersing agent ball milling mixing 12h, the volume of ceramic powder point in slurry
Number is 30%, and dispersing agent is polyacrylic acid, and the mass ratio of ceramic powder A and dispersing agent is 1:0.004~0.008, by deionization
Water, ceramic powder B and dispersing agent ball milling mixing 12h, the volume fraction of ceramic powder is 30% in slurry, and dispersing agent is polypropylene
The mass ratio of acid, ceramic powder B and dispersing agent is 1:0.004~0.008, and ceramic powder A is by α-Si3N4With sintering aid group
At sintering aid and α-Si3N4Mass ratio be 1:9, sintering aid is by Y2O3And Al2O3Powder composition, Y2O3And Al2O3's
Mass ratio is 1:0.6, and ceramic powder B is α-Si3N4;
Step 2: binder, plasticizer is added into mixed slurry A and mixed slurry B respectively, 30min is continuesd to mix, point
Casting slurry A and casting slurry B are not obtained, and binder is one of polyvinyl alcohol and acrylic emulsion, ceramic powder A or B
It is 1:0.004 with the mass ratio of bonding agent, plasticizer is glycerol, and the mass ratio of ceramic powder A or B and plasticizer is 1:0.008;
Step 3: casting slurry A and casting slurry B under vacuum conditions after de-bubble 20min, are poured on release film and carry out
Tape casting, molding scraper speed are 10cm/min, edge height 0.05mm, and the slurry after curtain coating is carried out at room temperature
12h is spontaneously dried, is then removed from release film, respectively obtains A layers of articulamentum of green compact and B layers of articulamentum of green compact;
Step 4: nitride porous silicon substrate I 1 and II 2 surface of nitride porous silicon substrate are polished with 800 mesh sand paper, it is rear with super
Sound washes and dries;
Step 5: by raw material in the way of I 1-A layers of-B layers of-A layers-nitride porous silicon substrate II 2 of nitride porous silicon substrate
It laminates and dumping, dump temperature is 600 DEG C in air, heating rate is 0.5 DEG C/min, and soaking time is 2 hours;
It is sintered Step 6: the raw material after laminating is placed in air pressure furnace, sintering temperature is 1700 DEG C, and soaking time is 3 small
When, nitrogen pressure 0.4MPa when sintering, passes through and places weight on nitride porous silicon substrate I 1 and nitride porous silicon substrate II 2
Object applies the pressure of 4MPa.
As seen from Figure 1, during the sintering process, growing up for the silicon nitride grain of articulamentum is to depend on two sides nitride porous
Silicon substrate I 1 and nitride porous silicon substrate II 2, and be not based on articulamentum itself, thus articulamentum do not occur during the sintering process it is bright
It is aobvious to shrink.If Fig. 2 can be seen that, it is sintered the later period, the silicon nitride grain of articulamentum is sufficiently grown up, mutually interspersed bridge joint, crystal grain ruler
It is very little similar to two sides nitride porous silicon substrate I 1 and nitride porous silicon substrate II 2 to draw ratio, therefore articulamentum has higher connection
Intensity.
Specific embodiment 4:
Illustrate that present embodiment, present embodiment are described further embodiment one below with reference to Fig. 1-2,
Step 1: by deionized water, ceramic powder A and dispersing agent ball milling mixing 12h, the volume of ceramic powder A in slurry
Score is 45%, and dispersing agent is one of polyacrylic acid and tetramethylammonium hydroxide, the mass ratio of ceramic powder A and dispersing agent
For 1:0.008, by deionized water, ceramic powder B and dispersing agent ball milling mixing 12h, the volume fraction of ceramic powder B is in slurry
45%, dispersing agent is one of polyacrylic acid and tetramethylammonium hydroxide, and the mass ratio of ceramic powder B and dispersing agent is 1:
0.008, ceramic powder A are by α-Si3N4It is formed with sintering aid, sintering aid and α-Si3N4Mass ratio be 1:19, sintering
Auxiliary agent is by Y2O3And Al2O3Powder composition, Y2O3And Al2O3Mass ratio be 1:0.8, ceramic powder B is α-Si3N4;
Step 2: binder, plasticizer is added into mixed slurry A and mixed slurry B respectively, 30min is continuesd to mix, point
Casting slurry A and casting slurry B are not obtained, and binder is one of polyvinyl alcohol and acrylic emulsion, ceramic powder A or B
Be 1:0.008 with the mass ratio of bonding agent, plasticizer is one or both of glycerol and polyethylene glycol, ceramic powder A or B with
The mass ratio of plasticizer is 1:0.016;
Step 3: being poured over release film for after casting slurry A and casting slurry B under vacuum conditions de-bubble 20min respectively
Upper carry out tape casting, molding scraper speed is 10cm/min, edge height 0.2mm, by the slurry after curtain coating in room temperature
Under carry out natural drying 12h, then removed from release film, respectively obtain A layers of articulamentum of green compact and B layers of articulamentum of life
Base;
Step 4: nitride porous silicon substrate I 1 and II 2 surface of nitride porous silicon substrate are polished with 1600 mesh sand paper, it is rear with super
Sound washes and dries;
Step 5: by raw material in the way of I 1-A layers of-B layers of-A layers-nitride porous silicon substrate II 2 of nitride porous silicon substrate
It laminates and dumping, dump temperature is 600 DEG C in air, heating rate is 0.3 DEG C/min, and soaking time is 4 hours;
It is sintered Step 6: the raw material after laminating is placed in air pressure furnace, sintering temperature is 1850 DEG C, soaking time 0.5
Hour, nitrogen pressure 1MPa when sintering, passes through and places weight on nitride porous silicon substrate I 1 and nitride porous silicon substrate II 2
Object applies the pressure of 0.5MPa.
As seen from Figure 1, during the sintering process, growing up for the silicon nitride grain of articulamentum is to depend on two sides nitride porous
Silicon substrate I 1 and nitride porous silicon substrate II 2, and be not based on articulamentum itself, thus articulamentum do not occur during the sintering process it is bright
It is aobvious to shrink.If Fig. 2 can be seen that, it is sintered the later period, the silicon nitride grain of articulamentum is sufficiently grown up, mutually interspersed bridge joint, crystal grain ruler
It is very little similar to two sides nitride porous silicon substrate I 1 and nitride porous silicon substrate II 2 to draw ratio, therefore articulamentum has higher connection
Intensity.
Certainly, above description is not limitation of the present invention, and the present invention is also not limited to the example above, the art
The variations, modifications, additions or substitutions that those of ordinary skill is made within the essential scope of the present invention also belong to guarantor of the invention
Protect range.
Claims (10)
1. a kind of connection method of porous silicon nitride ceramic, including nitride porous silicon substrate I (1), articulamentum and porous silicon nitride
Matrix II (2), it is characterised in that: the articulamentum is by being sintered nitride porous silicon substrate I (1) and nitride porous silicon substrate II
(2) it is connected with each other, articulamentum grows the nitride porous silicon substrate I (1) and nitride porous silicon substrate II (2) for depending on two sides, raw
The nitride porous silicon substrate I (1) and nitride porous silicon substrate II (2) of the mutually interspersed bridge joint two sides of articulamentum after length.
2. a kind of connection method of porous silicon nitride ceramic according to claim 1, it is characterised in that: the articulamentum by
Tri- layers of raw material of A-B-A laminate composition, and wherein A layers of the articulamentum of two sides is made of ceramic powder A, and ceramic powder A is by α-Si3N4With
Sintering aid composition, is made wherein being located in the middle B layers of articulamentum of ceramic powder B, ceramic powder B is by α-Si3N4Composition.
3. a kind of connection method of porous silicon nitride ceramic according to claim 2, it is characterised in that: described two sides A layers
Interior α-Si3N4Mass ratio with sintering aid is 1:9~19.
4. a kind of connection method of porous silicon nitride ceramic according to claim 3, it is characterised in that: the sintering aid
By Y2O3And Al2O3Powder composition, Y2O3And Al2O3Mass ratio be 1:0.6~0.8.
5. a kind of connection method of porous silicon nitride ceramic according to claim 2, it is characterised in that: the articulamentum
Green compact are prepared by tape casting, and specific preparation process includes the following steps:
Step 1: deionized water, ceramic powder A and dispersing agent ball milling mixing are prepared into mixed slurry A;
Step 2: deionized water, ceramic powder B and dispersing agent ball milling mixing are prepared into mixed slurry B;
Step 3: being separately added into binder, plasticizer in mixed slurry A and mixed slurry B, continuess to mix and respectively obtains curtain coating slurry
Expect A and casting slurry B;
Step 4: casting slurry A and casting slurry B after de-bubble, is poured on release film under vacuum conditions and carries out tape casting,
Slurry after curtain coating is spontaneously dried at room temperature, is then removed from release film, A layers of articulamentum of green compact are respectively obtained
With B layers of green compact of articulamentum.
6. a kind of connection method of porous silicon nitride ceramic according to claim 5, it is characterised in that: the binder is
In polyvinyl alcohol or acrylic emulsion, the mass ratio of ceramic powder and bonding agent is 1:0.004~0.008, and plasticizer is glycerol
One or both of with polyethylene glycol, the mass ratio of ceramic powder and plasticizer is 1:0.008~0.016.
7. a kind of connection method of porous silicon nitride ceramic according to any one of claims 1 to 6, it is characterised in that: institute
The matrix surface for stating nitride porous silicon substrate I (1) and nitride porous silicon substrate II (2) is both needed to be polished with sand paper, with super after polishing
Sound washes and dries.
8. a kind of connection method of porous silicon nitride ceramic according to any one of claims 1 to 6, it is characterised in that: In
By nitride porous silicon substrate I (1), articulamentum and nitride porous silicon substrate II (2) according to along nitride porous silicon substrate before sintering connection
Body I (1)-articulamentum-nitride porous silicon substrate II (2) sequence sequence stacks and dumping in air.
9. a kind of connection method of porous silicon nitride ceramic according to any one of claims 1 to 6, it is characterised in that: institute
State and be sintered to gas pressure sintering, sintering temperature be 1700~1850 DEG C, soaking time be 0.5~3 hour, nitrogen pressure be 0.4~
1MPa。
10. a kind of connection method of porous silicon nitride ceramic according to claim 9, it is characterised in that: when the sintering
The pressure of 0.5~4MPa need to be applied on nitride porous silicon substrate I (1) and nitride porous silicon substrate II (2).
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910908744.6A CN110483091B (en) | 2019-09-25 | 2019-09-25 | Connection method of porous silicon nitride ceramic |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910908744.6A CN110483091B (en) | 2019-09-25 | 2019-09-25 | Connection method of porous silicon nitride ceramic |
Publications (2)
Publication Number | Publication Date |
---|---|
CN110483091A true CN110483091A (en) | 2019-11-22 |
CN110483091B CN110483091B (en) | 2021-07-13 |
Family
ID=68544264
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910908744.6A Active CN110483091B (en) | 2019-09-25 | 2019-09-25 | Connection method of porous silicon nitride ceramic |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110483091B (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113956052A (en) * | 2021-11-15 | 2022-01-21 | 广东省科学院新材料研究所 | Forming method of ceramic microchannel, ceramic microchannel material and application |
CN116410019A (en) * | 2022-01-05 | 2023-07-11 | 北京小米移动软件有限公司 | Manufacturing method of ceramic piece, ceramic piece and electronic equipment |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
RU2365564C1 (en) * | 2008-01-28 | 2009-08-27 | Федеральное государственное унитарное предприятие "Обнинское научно-производственное предприятие "Технология" | Method of connecting ceramic units from silicon nitride |
CN107857595A (en) * | 2017-11-29 | 2018-03-30 | 上海大学 | Silicon nitride ceramics slurry and preparation method thereof and the application for preparing Silicon Nitride Slips by Tape Casting |
CN108147671A (en) * | 2017-12-28 | 2018-06-12 | 哈尔滨工业大学 | It is a kind of for devitrified glass solder of connecting silicon nitride ceramics and preparation method thereof |
CN108299004A (en) * | 2018-02-06 | 2018-07-20 | 中国科学院上海硅酸盐研究所 | A method of alleviating porous silicon nitride ceramic and transparent aluminium oxynitride ceramic joining process thermal stress |
CN108640522A (en) * | 2018-06-12 | 2018-10-12 | 哈尔滨工业大学 | A kind of devitrified glass solder and the method using solder welding porous silicon nitride and compact silicon nitride |
-
2019
- 2019-09-25 CN CN201910908744.6A patent/CN110483091B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
RU2365564C1 (en) * | 2008-01-28 | 2009-08-27 | Федеральное государственное унитарное предприятие "Обнинское научно-производственное предприятие "Технология" | Method of connecting ceramic units from silicon nitride |
CN107857595A (en) * | 2017-11-29 | 2018-03-30 | 上海大学 | Silicon nitride ceramics slurry and preparation method thereof and the application for preparing Silicon Nitride Slips by Tape Casting |
CN108147671A (en) * | 2017-12-28 | 2018-06-12 | 哈尔滨工业大学 | It is a kind of for devitrified glass solder of connecting silicon nitride ceramics and preparation method thereof |
CN108299004A (en) * | 2018-02-06 | 2018-07-20 | 中国科学院上海硅酸盐研究所 | A method of alleviating porous silicon nitride ceramic and transparent aluminium oxynitride ceramic joining process thermal stress |
CN108640522A (en) * | 2018-06-12 | 2018-10-12 | 哈尔滨工业大学 | A kind of devitrified glass solder and the method using solder welding porous silicon nitride and compact silicon nitride |
Non-Patent Citations (2)
Title |
---|
解荣军等: "氮化硅陶瓷连接工艺及结合强度研究", 《硅酸盐学报》 * |
解荣军等: "焊料中氮化硅含量对氮化硅陶瓷连接强度的影响", 《硅酸盐学报》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113956052A (en) * | 2021-11-15 | 2022-01-21 | 广东省科学院新材料研究所 | Forming method of ceramic microchannel, ceramic microchannel material and application |
CN116410019A (en) * | 2022-01-05 | 2023-07-11 | 北京小米移动软件有限公司 | Manufacturing method of ceramic piece, ceramic piece and electronic equipment |
Also Published As
Publication number | Publication date |
---|---|
CN110483091B (en) | 2021-07-13 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN111620711B (en) | Bionic silicon nitride ceramic material and preparation method thereof | |
CN109987944B (en) | High-thermal-conductivity silicon nitride ceramic substrate and preparation method thereof | |
CN106699209B (en) | The preparation method of continuous alumina fiber enhancing alumina ceramic-base composites | |
CN110483091A (en) | A kind of connection method of porous silicon nitride ceramic | |
JP5492208B2 (en) | Method for producing non-adhesive film mainly composed of silicon carbide | |
CN113087531B (en) | High-strength high-thermal-conductivity silicon nitride ceramic substrate and preparation method and application thereof | |
CN103708846B (en) | Preparation method of C/C-SiC composite material | |
CN103833403B (en) | The preparation method of the toughness reinforcing boron carbide ceramics matrix material of a kind of silicon carbide whisker and product | |
CN108585684A (en) | A kind of cement base Ceramic Tiles adhesive | |
CN106588074A (en) | Method for preparation of gradient porous ceramic by process combining slip casting and vacuum foaming | |
CN105272263B (en) | A kind of aqueous tape casting method preparing the carbon containing porous biscuit of silicon carbide reaction-sintered | |
CN108975937B (en) | Ceramic hollow buoyancy ball and manufacturing method thereof | |
CN106380207A (en) | Preparation method for aluminum nitride substrate | |
CN110922080A (en) | Modified recycled coarse aggregate, permeable water-storing concrete and preparation method thereof | |
CN111004020A (en) | Method for preparing high-purity alumina ceramic substrate at low temperature | |
CN104924412B (en) | The connection method of reaction sintering silicon carbide ceramic biscuit | |
CN114956828B (en) | Silicon carbide ceramic and preparation method and application thereof | |
CN108947392A (en) | A kind of high-elastic mould essence house ornamentation decoration mortar of low-carbon environment-friendly and preparation method thereof | |
CN115231903A (en) | Preparation process of large-size high-purity ceramic substrate | |
CN109336562B (en) | Preparation method of alumina-based ceramic composite material | |
US6494979B1 (en) | Bonding of thermal tile insulation | |
CN102276288B (en) | Preparation method of honeycomb ceramic having outer skin | |
CN110723964B (en) | Barrier layer, sintering mold and preparation method thereof | |
CN113716951A (en) | Preparation method of YAG-based transparent ceramic with large-size sheet composite structure | |
JP5189712B2 (en) | AlN substrate and manufacturing method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |