CN103922748A - Preparation method for porous silicon nitride ceramic - Google Patents
Preparation method for porous silicon nitride ceramic Download PDFInfo
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- CN103922748A CN103922748A CN201410095989.9A CN201410095989A CN103922748A CN 103922748 A CN103922748 A CN 103922748A CN 201410095989 A CN201410095989 A CN 201410095989A CN 103922748 A CN103922748 A CN 103922748A
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Abstract
The invention provides a preparation method for porous silicon nitride ceramic. The preparation method comprises the following steps: preparation of gel; addition of a pore forming agent; molding of a green body; drying of the green body; sintering of the green body; etc. The method combines a gel-casting and a pore forming agent addition process together and has the advantages of simple process, low cost and substantially shortened gel discharge time; and the prepared porous silicon nitride ceramic has great porosity, high bending strength and good mechanical properties.
Description
Technical field
The invention belongs to material science, particularly a kind of gel injection and the method for interpolation pore-forming material legal system for porous silicon nitride ceramic of merging.
Background technology
Porous silicon-nitride ceramic material is a kind of function and structure integration stupalith, not only has the functional of porous ceramics, as good in dielectric properties, wideband perviousness uniformly, bigger serface etc.; And there is the functional of silicon nitride ceramics, and such as porosity is high, flexural strength is large, high temperature resistant, wear-resistant, anti-weathering, and thermal shock resistance is good etc.
Due to the over-all properties of porous silicon-nitride ceramic material excellence, be widely used in the fields such as petrochemical complex, metallurgical machinery, biological medicine, space flight and aviation, especially along with the fast development of field of aerospace in recent years, make porous silicon-nitride ceramic material become one of focus space material of vast researcher research.
The preparation method of existing porous silicon nitride ceramic conventionally adopts gel injection method and adds pore-forming material method.As clean in Chinese patent ZL201110181203.1(Wang Hong; Li Liuyuan; Champion Qiao; Yang Jianfeng, trimethyl carbinol base gel injection legal system is for the forming method of Si<sub>3</subGre atT.GreaT.GTN<sub>4LEssT.LTss T.LT/sub> porous ceramics) a kind of non-water base gel injection of openly knowing clearly prepares a method for porous silicon nitride ceramic, and Chinese patent ZL200910021515.9(Wang Hong is clean; Yu Juanli; Zhang Jian etc., a kind of method of gel injection legal system for porous SiN ceramic of utilizing) a kind of gel injection of openly knowing clearly prepares the method for porous silicon nitride ceramic.But above method has all adopted single gel injection method, the porous silicon nitride ceramic intensity that makes is low, dry environment is complicated, binder removal process time is longer.And while adding pore-forming material legal system for porous silicon nitride ceramic, all need to adopt the technique of pressed compact moulding, therefore cause product porosity.
Summary of the invention
Goal of the invention: in order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of gel injection and the method for interpolation pore-forming material legal system for porous silicon nitride ceramic of merging, utilize the method can make fast porous silicon nitride ceramic, and the porous silicon nitride ceramic intensity making is high, excellent combination property.
Technical scheme: the preparation method of a kind of porous silicon nitride ceramic provided by the invention, comprises the following steps:
(1) preparation of gel: softening agent, monomer, linking agent and deionized water are mixed, obtain premixed liquid; In premixed liquid, add dispersion agent, beta-silicon nitride powder and sintering aid, tune pH is 8-12, and ball milling 4-15h, obtains gel;
(2) add pore-forming material: gel and pore-forming material are mixed;
(3) moulding of base substrate: the gel that step (2) is added to pore-forming material, after vacuum stripping, adds initiator and catalyzer to mix, casting after vacuum stripping, room temperature reaction 20-50min makes the demoulding of gel crosslinking curing, obtains idiosome;
(4) base substrate is dry: base substrate seasoning 10-15 days is to constant weight;
(5) binder removal of base substrate: idiosome binder removal in chamber type electric resistance furnace that step (4) is dry; Binder removal condition is: room temperature taking temperature rise rate as 0.5-1 DEG C/min is warming up to 150 DEG C, then from 150 DEG C taking temperature rise rate as 0.2-0.5 DEG C/min is warming up to 600 DEG C, and is incubated 1-2h respectively in the time of 100 DEG C, 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C; Cooling;
(6) sintering of base substrate: the base substrate sintering in nitrogen atmosphere after step (5) binder removal, sintering condition is: room temperature is warming up to 1700-1800 DEG C with the speed of 5-15 DEG C/min, insulation 1-3h, furnace cooling, to obtain final product.
As preferably, the weight ratio of described softening agent, monomer, linking agent, deionized water, dispersion agent, beta-silicon nitride powder, sintering aid, pore-forming material, initiator, catalyzer is (1-3): (10-20): (2-3): 100:(0.4-0.6): (90-100): (4-6): (0.1-30): (0.08-0.10): (0.4-0.6), be preferably 2:15:2.5:100:0.5:95:5:15:0.09:0.5.
Preferred as another kind, described softening agent is polyacrylamide, preferably the polyacrylamide of molecular-weight average more than 3000000.
Preferred as another kind, described monomer is acrylamide, and described linking agent is N, N '-methylene-bisacrylamide.
Preferred as another kind, described dispersion agent is ammonium polyacrylate, the ammonium polyacrylate that preferably molecular-weight average is 3000-5000.
Preferred as another kind, described sintering aid is that mass ratio is (4-6): 2 yttrium oxide and the mixture of aluminum oxide, preferred mass is than being the yttrium oxide of 5:2 and the mixture of aluminum oxide.
Preferred as another kind, described pore-forming material is alumina hollow ball, and preferably median size is the alumina hollow ball of 50-100 μ m.
Preferred as another kind, described initiator is ammonium persulphate, and catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine.
Preferred as another kind, described porous silicon nitride ceramic porosity is 44.98-61.19%, and flexural strength is 78.93-125.07MPa, and fracture toughness property is 1.40-2.38MPa.m
1/2.
Beneficial effect: the preparation method of porous silicon nitride ceramic provided by the invention adopts gel injection method and adds the combination of pore-forming material method, technique is simple, cost is low, the binder removal time shortens greatly, and the porous silicon nitride ceramic porosity that makes is large, flexural strength is high, mechanical property good.The porosity of the porous silicon nitride ceramic that employing the method makes is 44.98%-61.19%, and flexural strength is 78.93-125.07MPa, and fracture toughness property is 1.40～2.38MPa.m
1/2.Meanwhile, the method can be prepared large size, complex-shaped porous ceramic member.
Specifically, the present invention, with respect to prior art, has following outstanding advantage:
(1) the present invention effectively combines gel injection method and interpolation pore-forming material method, forms a kind of preparation method of novel porous silicon nitride ceramic, and technique is simple, the time is short, efficiency is high, cost is low, can realize large size moulding and complex parts moulding.
(2) the method condition is easily controlled, and in blank forming process, can control by controlling the add-on of initiator and catalyzer the set time of gel.
(3) the method drying process is carried out under room temperature environment, convenient and simple, and the binder removal time is short, and production efficiency is high.
(4) the porous silicon nitride ceramic porosity that adopts the method to prepare is large, and flexural strength is high, mechanical property excellence.
Brief description of the drawings
Fig. 1 is the SEM photo of the porous silicon nitride ceramic fracture apperance that makes of the inventive method.
Fig. 2 is pore-forming material addition and the porosity of flexural strength and porous silicon nitride ceramic and the graph of a relation of fracture toughness property.
Fig. 3 is the XRD figure spectrum of the porous silicon nitride ceramic that makes of the inventive method.
Embodiment
Embodiment 1
The preparation of porous silicon nitride ceramic, comprises the following steps:
(1) preparation of gel: by the softening agent of 2 weight parts, the monomer of 15 weight parts, the linking agent of 2.5 weight parts, mixes with the deionized water of 100 weight parts, prepares premixed liquid; In premixed liquid, add the dispersion agent of 0.5 weight part, the sintering aid of the beta-silicon nitride powder of 95 weight parts and 5 weight parts, regulating PH is 8, then ball milling prepares gel after 4 hours;
(2) add pore-forming material: in the gel of preparation, add the pore-forming material of 15 weight parts, and machinery stirs;
(3) moulding of base substrate: add the slurry of pore-forming material through vacuum stripping, add the initiator of 0.08 weight part and the catalyzer of 0.5 weight part, casting after vacuum stripping again, at ambient temperature, react the then demoulding of gel generation crosslinking curing after 50 minutes, obtain idiosome;
(4) base substrate is dry: the base substrate after the demoulding is placed under room temp and humidity condition, and seasoning 10 days, in the time that the quality of base substrate no longer changes, body drying completes;
(5) binder removal of base substrate: the whole process of base substrate binder removal is carried out in chamber type electric resistance furnace.In binder removal process, from room temperature to 150 DEG C, temperature rise rate is 0.6 DEG C/min, and from 150 DEG C～600 DEG C, temperature rise rate is 0.3 DEG C/min, and respectively 100 DEG C, 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C each insulations one hour;
(6) sintering of base substrate: the base substrate after binder removal is sintering in normal pressure nitrogen atmosphere, be warming up to 1750 DEG C from room temperature with the speed of 10 DEG C/min, be incubated furnace cooling after 2 hours, the porosity of the porous silicon nitride ceramic finally obtaining is 61.19%, flexural strength is 100.83MPa, and fracture toughness property is 1.58MPa.m
1/2.
Wherein, described softening agent is the polyacrylamide of molecular-weight average 3000000; Described monomer is acrylamide, and described linking agent is N, N '-methylene-bisacrylamide; Dispersion agent is that molecular-weight average is 4000 ammonium polyacrylate; Sintering aid is that mass ratio is the yttrium oxide of 5:2 and the mixture of aluminum oxide; Described pore-forming material is that median size is the alumina hollow ball of 80 μ m; Described initiator is ammonium persulphate; Catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine.
Embodiment 2
The preparation of porous silicon nitride ceramic, comprises the following steps:
(1) preparation of gel: by the softening agent of 2 weight parts, the monomer of 15 weight parts, the linking agent of 2.5 weight parts, mixes with the deionized water of 100 weight parts, prepares premixed liquid; In premixed liquid, add the dispersion agent of 0.5 weight part, the sintering aid of the beta-silicon nitride powder of 95 weight parts and 5 weight parts, regulating PH is 9, then ball milling prepares gel after 8 hours;
(2) add pore-forming material: in the gel of preparation, add the pore-forming material of 5 weight parts, and mechanical stirring, pore-forming material is evenly distributed in gel;
(3) moulding of base substrate: add the slurry of pore-forming material through vacuum stripping, add the initiator of 0.08 weight part and the catalyzer of 0.5 weight part, casting after vacuum stripping again, at ambient temperature, react the then demoulding of gel generation crosslinking curing after 50 minutes, obtain idiosome;
(4) base substrate is dry: the base substrate after the demoulding is placed under room temp and humidity condition, and seasoning 13 days, in the time that the quality of base substrate no longer changes, body drying completes;
(5) binder removal of base substrate: the whole process of base substrate binder removal is carried out in chamber type electric resistance furnace.In binder removal process, from room temperature to 150 DEG C, temperature rise rate is 0.8 DEG C/min, and from 150 DEG C～600 DEG C, temperature rise rate is 0.4 DEG C/min, and respectively 100 DEG C, 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C each insulations one hour;
(6) sintering of base substrate: the base substrate after binder removal is sintering in normal pressure nitrogen atmosphere, be warming up to 1750 DEG C from room temperature with the speed of 5 DEG C/min, be incubated furnace cooling after 2 hours, the porosity of the porous silicon nitride ceramic finally obtaining is 51.02%, flexural strength is 112.05MPa, and fracture toughness property is 2.15MPa.m
1/2.
Wherein, described softening agent is the polyacrylamide of molecular-weight average 3000000; Described monomer is acrylamide, and described linking agent is N, N '-methylene-bisacrylamide; Dispersion agent is that molecular-weight average is 4000 ammonium polyacrylate; Sintering aid is that mass ratio is the yttrium oxide of 5:2 and the mixture of aluminum oxide; Described pore-forming material is that median size is the alumina hollow ball of 60 μ m; Described initiator is ammonium persulphate; Catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine.
Embodiment 3
The preparation of porous silicon nitride ceramic, comprises the following steps:
(1) preparation of gel: by the softening agent of 2 weight parts, the monomer of 15 weight parts, the linking agent of 2.5 weight parts, mixes with the deionized water of 100 weight parts, prepares premixed liquid; In premixed liquid, add the dispersion agent of 0.5 weight part, the sintering aid of the beta-silicon nitride powder of 95 weight parts and 5 weight parts, regulating PH is 11, then ball milling prepares gel after 12 hours;
(2) add pore-forming material: in the gel of preparation, add the pore-forming material of 10 weight parts, and mechanical stirring, pore-forming material is evenly distributed in gel;
(3) moulding of base substrate: add the slurry of pore-forming material through vacuum stripping, add the initiator of 0.09 weight part and the catalyzer of 0.5 weight part, casting after vacuum stripping again, at ambient temperature, react the then demoulding of gel generation crosslinking curing after 40 minutes, obtain idiosome;
(4) base substrate is dry: the base substrate after the demoulding is placed under room temp and humidity condition, and seasoning 14 days, in the time that the quality of base substrate no longer changes, body drying completes;
(5) binder removal of base substrate: the whole process of base substrate binder removal is carried out in chamber type electric resistance furnace.In binder removal process, from room temperature to 150 DEG C, temperature rise rate is 0.7 DEG C/min, and from 150 DEG C～600 DEG C, temperature rise rate is 0.4 DEG C/min, and respectively 100 DEG C, 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C each insulations one hour;
(6) sintering of base substrate: the base substrate after binder removal is sintering in normal pressure nitrogen atmosphere, be warming up to 1750 DEG C from room temperature with the speed of 10 DEG C/min, be incubated furnace cooling after 2 hours, the porosity of the porous silicon nitride ceramic finally obtaining is 48.25%, flexural strength is 125.07MPa, and fracture toughness property is 2.38MPa.m
1/2.
Wherein, described softening agent is the polyacrylamide of molecular-weight average 3000000; Described monomer is acrylamide, and described linking agent is N, N '-methylene-bisacrylamide; Dispersion agent is that molecular-weight average is 4000 ammonium polyacrylate; Sintering aid is that mass ratio is the yttrium oxide of 5:2 and the mixture of aluminum oxide; Described pore-forming material is that median size is the alumina hollow ball of 80 μ m; Described initiator is ammonium persulphate; Catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine.
Embodiment 4
The preparation of porous silicon nitride ceramic, comprises the following steps:
(1) preparation of gel: by the softening agent of 1 weight part, the monomer of 10 weight parts, the linking agent of 2 weight parts, mixes with the deionized water of 100 weight parts, prepares premixed liquid; In premixed liquid, add the dispersion agent of 0.4 weight part, the sintering aid of the beta-silicon nitride powder of 90 weight parts and 4 weight parts, regulating pH is 8, then ball milling prepares gel after 15 hours;
(2) add pore-forming material: in the gel of preparation, add the pore-forming material of 0.1 weight part, and mechanical stirring, pore-forming material is evenly distributed in gel;
(3) moulding of base substrate: add the slurry of pore-forming material through vacuum stripping, add the initiator of 0.08 weight part and the catalyzer of 0.4 weight part, casting after vacuum stripping again, at ambient temperature, react the then demoulding of gel generation crosslinking curing after 50 minutes, obtain idiosome;
(4) base substrate is dry: the base substrate after the demoulding is placed under room temp and humidity condition, and seasoning 15 days, in the time that the quality of base substrate no longer changes, body drying completes;
(5) binder removal of base substrate: the whole process of base substrate binder removal is carried out in chamber type electric resistance furnace.In binder removal process, from room temperature to 150 DEG C, temperature rise rate is 0.5 DEG C/min; From 150 DEG C～600 DEG C, temperature rise rate is 0.2 DEG C/min, and respectively at 100 DEG C, 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C each insulation 1h;
(6) sintering of base substrate: the base substrate after binder removal is sintering in normal pressure nitrogen atmosphere, be warming up to 1700 DEG C from room temperature with the speed of 10 DEG C/min, be incubated furnace cooling after 1 hour, the porosity of the porous silicon nitride ceramic finally obtaining is 44.98%, flexural strength is 78.96MPa, and fracture toughness property is 1.90MPa.m
1/2.
Wherein, described softening agent is the polyacrylamide of molecular-weight average 4000000; Described monomer is acrylamide, and described linking agent is N, N '-methylene-bisacrylamide; Dispersion agent is that molecular-weight average is 3000 ammonium polyacrylate; Sintering aid is that mass ratio is the yttrium oxide of 4:2 and the mixture of aluminum oxide; Described pore-forming material is that median size is the alumina hollow ball of 50 μ m; Described initiator is ammonium persulphate; Catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine.
Embodiment 5
The preparation of porous silicon nitride ceramic, comprises the following steps:
(1) preparation of gel: by the softening agent of 3 weight parts, the monomer of 20 weight parts, the linking agent of 3 weight parts, mixes with the deionized water of 100 weight parts, prepares premixed liquid; In premixed liquid, add the dispersion agent of 0.6 weight part, the sintering aid of the beta-silicon nitride powder of 100 weight parts and 6 weight parts, regulating pH is 12, then ball milling prepares gel after 12 hours;
(2) add pore-forming material: in the gel of preparation, add the pore-forming material of 30 weight parts, and mechanical stirring, pore-forming material is evenly distributed in gel;
(3) moulding of base substrate: add the slurry of pore-forming material through vacuum stripping, add the initiator of 0.10 weight part and the catalyzer of 0.6 weight part, casting after vacuum stripping again, at ambient temperature, react the then demoulding of gel generation crosslinking curing after 20 minutes, obtain idiosome;
(4) base substrate is dry: the base substrate after the demoulding is placed under room temp and humidity condition, and seasoning 13 days, in the time that the quality of base substrate no longer changes, body drying completes;
(5) binder removal of base substrate: the whole process of base substrate binder removal is carried out in chamber type electric resistance furnace.In binder removal process, from room temperature to 150 DEG C, temperature rise rate is 1 DEG C/min; From 150 DEG C～600 DEG C, temperature rise rate is 0.5 DEG C/min, and respectively at 100 DEG C, 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C each insulation 2h;
(6) sintering of base substrate: the base substrate after binder removal is sintering in normal pressure nitrogen atmosphere, be warming up to 1800 DEG C from room temperature with the speed of 15 DEG C/min, be incubated furnace cooling after 3 hours, the porosity of the porous silicon nitride ceramic finally obtaining is 45.12%, flexural strength is 78.93MPa, and fracture toughness property is 1.40MPa.m
1/2.
Wherein, described softening agent is the polyacrylamide of molecular-weight average 5000000; Described monomer is acrylamide, and described linking agent is N, N '-methylene-bisacrylamide; Dispersion agent is that molecular-weight average is 5000 ammonium polyacrylate; Sintering aid is that mass ratio is the yttrium oxide of 6:2 and the mixture of aluminum oxide; Described pore-forming material is that median size is the alumina hollow ball of 100 μ m; Described initiator is ammonium persulphate; Catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine.
Comparative example 1
Adopt gel injection legal system for porous silicon nitride ceramic, comprise the following steps:
(1) preparation of gel: by the softening agent of 2 weight parts, the monomer of 15 weight parts, the linking agent of 2.5 weight parts, mixes with the deionized water of 100 weight parts, prepares premixed liquid; In premixed liquid, add the dispersion agent of 0.5 weight part, the sintering aid of the beta-silicon nitride powder of 78 weight parts and 4 weight parts, regulating PH is 10, then ball milling prepares gel after 12 hours;
(2) moulding of base substrate: add the slurry of pore-forming material through vacuum stripping, add the initiator of 0.08 weight part and the catalyzer of 0.5 weight part, casting after vacuum stripping again, at ambient temperature, react the then demoulding of gel generation crosslinking curing after 30 minutes, obtain idiosome;
(3) base substrate is dry: the base substrate after the demoulding is placed under room temp and humidity condition, and seasoning 13 days, in the time that the quality of base substrate no longer changes, body drying completes;
(4) binder removal of base substrate: the whole process of base substrate binder removal is carried out in chamber type electric resistance furnace.In binder removal process, from room temperature to 150 DEG C, temperature rise rate is 1 DEG C/min, and from 150 DEG C～600 DEG C, temperature rise rate is 0.5 DEG C/min, and respectively 100 DEG C, 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C each insulations one hour;
(5) sintering of base substrate: the base substrate after binder removal is sintering in normal pressure nitrogen atmosphere, be warming up to 1750 DEG C from room temperature with the speed of 10 DEG C/min, be incubated furnace cooling after 2 hours, the porosity of the porous silicon nitride ceramic finally obtaining is 63.26%, flexural strength is 96.67MPa, and fracture toughness property is 1.54MPa.m
1/2.
Wherein, described softening agent is the polyacrylamide of molecular-weight average 3000000; Described monomer is acrylamide, and described linking agent is N, N '-methylene-bisacrylamide; Dispersion agent is that molecular-weight average is 4000 ammonium polyacrylate; Sintering aid is that mass ratio is the yttrium oxide of 5:2 and the mixture of aluminum oxide; Described initiator is ammonium persulphate; Catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine.
Comparative example 2
Adopt and add pore-forming material legal system for porous silicon nitride ceramic, comprise the following steps:
(1) mixed powder: by the silicon nitride powder of 93 weight parts, the yttrium oxide of 5 weight parts, the aluminum oxide of 2 weight parts, mixes with dehydrated alcohol, then ball milling 12h;
(2) sieve: with Rotary Evaporators, powder mixed in (1) is dry, then with 120 object standard sieves, dry powder is sieved;
(3) add pore-forming material: in the powder after sieving, add the alumina hollow ball of 10 weight parts in (2), and machinery stirs;
(4) pressed compact: adopt omnipotent pressure testing machine by dry-pressing formed under 20MPa the powder in (3), then isostatic pressing under 150MPa, obtains biscuit;
(5) sintering: plain body is sintering in normal pressure nitrogen atmosphere, be warming up to 1750 DEG C from room temperature with the speed of 10 DEG C/min, be incubated furnace cooling after 2 hours, the porosity of the porous silicon nitride ceramic finally obtaining is 38.62%, flexural strength is 180.39MPa, and fracture toughness property is 2.67MPa.m1/2.
Can be found by comparative example and embodiment contrast, adopt the standby porous silicon nitride ceramic of gel injection legal system, it is higher that porosity can reach, but flexural strength and fracture toughness property are relatively low; Add and adopt the porous silicon nitride ceramic that pore-forming material method prepares, although that flexural strength and fracture toughness property can reach is higher, porosity is very little; And the present invention adopts gel injection method and add the combination of pore-forming material method, the porous silicon-nitride ceramic material preparing, porosity is high, and mechanical property is more excellent.
Claims (9)
1. a preparation method for porous silicon nitride ceramic, is characterized in that: comprise the following steps:
(1) preparation of gel: softening agent, monomer, linking agent and deionized water are mixed, obtain premixed liquid; In premixed liquid, add dispersion agent, beta-silicon nitride powder and sintering aid, tune pH is 8-12, and ball milling 4-15h, obtains gel;
(2) add pore-forming material: gel and pore-forming material are mixed;
(3) moulding of base substrate: the gel that step (2) is added to pore-forming material, after vacuum stripping, adds initiator and catalyzer to mix, casting after vacuum stripping, room temperature reaction 20-50min makes the demoulding of gel crosslinking curing, obtains idiosome;
(4) base substrate is dry: base substrate seasoning 10-15 days is to constant weight;
(5) binder removal of base substrate: idiosome binder removal in chamber type electric resistance furnace that step (4) is dry; Binder removal condition is: room temperature taking temperature rise rate as 0.5-1 DEG C/min is warming up to 150 DEG C, then from 150 DEG C taking temperature rise rate as 0.2-0.5 DEG C/min is warming up to 600 DEG C, and is incubated 1-2h respectively in the time of 100 DEG C, 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C; Cooling;
(6) sintering of base substrate: the base substrate sintering in nitrogen atmosphere after step (5) binder removal, sintering condition is: room temperature is warming up to 1700-1800 DEG C with the speed of 5-15 DEG C/min, insulation 1-3h, furnace cooling, to obtain final product.
2. the preparation method of a kind of porous silicon nitride ceramic according to claim 1, is characterized in that: the weight ratio of described softening agent, monomer, linking agent, deionized water, dispersion agent, beta-silicon nitride powder, sintering aid, pore-forming material, initiator, catalyzer is (1-3): (10-20): (2-3): 100:(0.4-0.6): (90-100): (4-6): (0.1-30): (0.08-0.10): (0.4-0.6).
3. the preparation method of a kind of porous silicon nitride ceramic according to claim 1, is characterized in that: described softening agent is polyacrylamide, preferably the polyacrylamide of molecular-weight average more than 3000000.
4. the preparation method of a kind of porous silicon nitride ceramic according to claim 1, is characterized in that: described monomer is acrylamide, and described linking agent is N, N '-methylene-bisacrylamide.
5. the preparation method of a kind of porous silicon nitride ceramic according to claim 1, is characterized in that: described dispersion agent is ammonium polyacrylate, the ammonium polyacrylate that preferably molecular-weight average is 3000-5000.
6. the preparation method of a kind of porous silicon nitride ceramic according to claim 1, is characterized in that: described sintering aid is that mass ratio is (4-6): 2 yttrium oxide and the mixture of aluminum oxide.
7. the preparation method of a kind of porous silicon nitride ceramic according to claim 1, is characterized in that: described pore-forming material is alumina hollow ball, and preferably median size is the alumina hollow ball of 50-100 μ m.
8. the preparation method of a kind of porous silicon nitride ceramic according to claim 1, is characterized in that: described initiator is ammonium persulphate, and catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine.
9. the preparation method of a kind of porous silicon nitride ceramic according to claim 1, is characterized in that: described porous silicon nitride ceramic porosity is 44.98-61.19%, and flexural strength is 78.93-125.07MPa, and fracture toughness property is 1.40-2.38MPa.m
1/2.
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| CN103496999A (en) * | 2013-09-18 | 2014-01-08 | 清华大学 | Method for preparing porous ceramics from hollow ceramic ball |
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