CN102351563A - Preparation method for silicon nitride porous ceramic with multilevel pore size structure and high porosity - Google Patents
Preparation method for silicon nitride porous ceramic with multilevel pore size structure and high porosity Download PDFInfo
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Abstract
The invention provides a preparation method for a silicon nitride porous ceramic with a multilevel pore size structure and high porosity. The method comprises the following steps: uniformly mixing slurry of alpha-silicon nitride and diluent of an organic silicon resin, wherein, the volume ratio of alpha-silicon nitride to the organic silicon resin is 1:9 to 4:1; carrying out drying, ball milling and sieving on an obtained mixture, and uniformly mixing the mixture with naphthalene powder according to a mass ratio of 19:1 to 1:1; carrying out compression molding on obtained mixed powder, or carrying out isostatic pressing after molding of the obtained mixed powder; carrying out binder removal on a formed sample for 12 to 24 h at a temperature of 50 to 130 DEG C in a gradient heating mode; sintering a resultant of heat treatment at a temperature of 1100 to 1700 DEG C in a nitrogen atmosphere under normal pressure with insulation time being 1 to 5 h so as to obtain the silicon nitride porous ceramic. The invention has the advantages of a simple process, low cost and good repeatability; the prepared silicon nitride porous ceramic has excellent performance, e.g. wide pore size distribution, uniform pore distribution, high porosity and good mechanical strength.
Description
Technical field
The invention belongs to the stupalith field, particularly a kind of preparation method with high porosity porous SiN ceramic of multistage aperture structure.
Background technology
Along with the development of science and technology and suitability for industrialized production, problems such as the energy, resource, the disposal of three wastes come into one's own more.Especially high-tech sectors such as biochemical industry, fine chemistry industry, energy and material develops rapidly; Liquid, solid Research of Separation Technique and exploitation are proposed higher requirement, and high score more and more causes people's attention from the porous filtering technology and the porous filter material of precision, high operational efficiency.
Porous ceramic film material is meant through high-temperature firing and forms, and has in the body to communicate or the stupalith of closed pore.Porous ceramic film material is as one type of novel structure/function integration material; Because have that volume density is little, porosity is high, air permeance resistance is little, controllable bore diameter, cleaning and regeneration be convenient; Characteristics such as especially high temperature resistant, high pressure, resistant to chemical media corrosion have bigger application in a lot of fields.Ceramic filter technology and the ceramic filter device of doing filtration medium with porous ceramic film material have not only solved sad filter problems such as high temperature, high pressure, strong acid-base and chemical solvents medium; And because filtering accuracy itself that have is high, clean state is good and characteristics such as easy cleaning, long service life; Therefore, be used widely in fields such as oil, chemical industry, pharmacy, food, environmental protection and water treatments at present.
The tradition solid-liquid separation is that its pore size distribution is narrower with the big problem that ceramic foam exists, and the solid particulate major part is deposited in the upper surface of filter material during solid-liquid separation, has not only influenced isolating speed, and needs often to clean.To this difficult problem, industry advocates to utilize the characteristics of multilevel hole material varying aperture to realize classified filtering.But the research of present multilevel hole material mainly be utilize the organic formwork method to realize micropore at molecular scale ((aperture is between (the combination in aperture＞50nm) of 2～50nm)-macropore in aperture＜2nm)-mesoporous; Its pore diameter range is confined to 0.001～1 μ m basically, does not see the report of pore diameter range in the preparation method of the porous ceramic film material of 0.1～500 μ m at present.Porous SiN ceramic with hierarchical porous structure provided by the invention has effectively been expanded pore diameter range (0.1～500 μ m), can realize the high efficiency separation of solid-liquid.
The present invention is matrix with the silicon nitride.Silicon nitride ceramics is one of over-all properties best material in the structural ceramics.Its decomposition temperature is 1900 ℃, has excellent high-temperature stability ability and chemical stability; Through the α transformation of β phase in opposite directions, its flexural strength can reach about 1Gpa, has good mechanical property; Its specific inductivity is about 7.0, and loss tangent is about 0.004, has good electric property.In view of silicon nitride ceramics excellent heat, power, electric over-all properties; Can the porous silicon nitride ceramic of high porosity be applied to strainer, decontaminating separator, chemical industry catalytic carrier, transmitter under high temperature, high pressure, the acid etching condition etc., the porous silicon nitride ceramic of low porosity is applied to high temperature member.And through the control of electrical design and porosity, but also porous silicon nitride ceramic is applied to ripple field thoroughly such as missile-borne radome.
Silicone resin is a kind of cheapness, has the ceramic first body of better adhesive property and pore-creating performance that the Si-O-C structure that forms during its cracking at high temperature can play good enhancement.The fusing point of naphthalene is 80.5 ℃, is subliming type pore-forming material a kind of cheapness, excellent property.
The present invention adopts the normal pressure-sintered technology of atmosphere protection, is that matrix, silicone resin are that sticker and aperture pore-forming material, naphthalene powder are the macropore pore-forming material with the silicon nitride, prepares the high porosity porous SiN ceramic with multistage aperture structure.
Summary of the invention
Technical problem to be solved by this invention is: the method that the high porosity porous SiN ceramic that a kind of preparation has multistage aperture structure is provided.
The present invention solves its technical problem and adopts following technical scheme:
Preparing method with high porosity porous SiN ceramic of multistage aperture structure provided by the invention, be a kind of be sticker and aperture pore-forming material, naphthalene powder with the silicone resin for the macropore pore-forming material prepares the method for porous SiN ceramic, its step comprises:
(1) coats: the α-Dan Huagui powder is mixed with ethanol, obtain the α-Dan Huagui slip; Silicone resin is mixed with toluene, obtain the silicone resin dilute solution; α-Dan Huagui slip and silicone resin dilute solution are mixed, obtain mixed slurry, wherein the volume ratio of α-Dan Huagui and pure silicone resin is 1:9～4:1, and mixing time is 6～24h; Containing the α-Dan Huagui volume(tric)fraction in the α-Dan Huagui slip is 10～80%, and the silicone resin volume(tric)fraction is 10～50% in the silicone resin dilute solution;
(2) pre-treatment: at 80～120 ℃ of drying 12～24h, the gained solid sieves behind ball milling, obtains coated powder with mixed slurry;
(3) mix: the coated powder and the naphthalene powder of gained are mixed, obtain mixed powder;
(4) moulding: with mixed powder compression molding or mold pressing continued cold isostatic compaction, forming pressure is 10～400MPa, obtains the moulding sample;
(5) binder removal: employing ladder-elevating temperature pattern at 50～130 ℃ of binder removal 12～24h, obtains biscuit with the moulding sample;
(6) cracking: biscuit is normal pressure-sintered under 1100～1700 ℃, nitrogen atmosphere, and temperature rise rate is 0.5～10 ℃/min, and soaking time is 1～5h, promptly obtains said high porosity porous SiN ceramic with multistage aperture structure.
Described multistage aperture structure is meant that the porous SiN ceramic pore diameter range contains 0.1～500 μ m, is multistage distribution.
Described porous SiN ceramic, its porosity are 25～75%.
In the described coated powder, the volume content of silicone resin is 20～90%.
The meta particle diameter of said α-Dan Huagui powder is 0.4～5 μ m.
The particle diameter of said coated powder≤100 μ m.Because be to sieve, so should be less than a certain numerical value.
The meta particle diameter of said naphthalene powder≤300 μ m.
In the described mixed powder, the mass ratio of coated powder and naphthalene powder is 19:1～1:1.
In moulding process, compression molding pressure is 10～150MPa; Or mold pressing continued cold isostatic compaction, forming pressure is 100～400MPa.
Described employing ladder-elevating temperature pattern, specifically: 50～70 ℃ of insulation 1～2h; Be warming up to 70～90 ℃ of insulation 8～16h; Be warming up to 90～110 ℃ of insulation 2～8h; Be warming up to 110～130 ℃ of insulation 1～4h at last.
The present invention compared with prior art has following major advantage:
1. simple, the favorable repeatability, with low cost of technology, and the porous SiN ceramic of preparation has excellent properties such as pore size distribution is wide, porosity is high, mechanical strength is good.
2. the pore diameter range of the porous SiN ceramic of preparation is 0.1～500 μ m, is multistage distribution, can be widely used in aspects such as classified filtering, stage purification, chemical industry catalytic carrier, sound absorption damping, senior lagging material, sensing material and electromagnetic wave transparent material.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is the XRD figure spectrum of embodiment 1 to embodiment 6 gained material.
Fig. 3 is the SEM image (50 times) of embodiment 1 to embodiment 4 gained material.
Fig. 4 is the SEM image (10000 times) of embodiment 1 to embodiment 5 gained material.
Fig. 5 is the SEM image (5000 times) of embodiment 3 gained materials.
Fig. 6 is the SEM image (50 times) of embodiment 5 gained materials.
Fig. 7 is the SEM image (50 times) of embodiment 6 gained materials.
Fig. 8 is the SEM image (10000 times) of embodiment 6 gained materials.
Embodiment
The present invention adopts the normal pressure-sintered technology of atmosphere protection; With the silicon nitride is that matrix, silicone resin are that sticker and pore-forming material, naphthalene powder are pore-forming material; Prepare high porosity porous SiN ceramic with multistage aperture structure; Be specially: the α-Dan Huagui powder is mixed with ethanol, obtain the α-Dan Huagui slip; Silicone resin is mixed with toluene, obtain the silicone resin dilute solution; α-Dan Huagui slip and silicone resin diluent are mixed, and wherein the volume ratio of α-Dan Huagui and silicone resin is 1:9～4:1; Gains mix with the naphthalene powder through super-dry, ball milling, after sieving, and the two mass ratio is 19:1～1:1; With cold isostatic compaction after mixed powder compression molding or the mold pressing; Adopt the ladder-elevating temperature pattern with the moulding sample at 50～130 ℃ of binder removal 12～24h; Product after the thermal treatment is normal pressure-sintered under 1100～1700 ℃, nitrogen atmosphere, and temperature rise rate is 0.5～10 ℃/min, and soaking time is 1～5h, promptly obtains a kind of porous SiN ceramic with multistage aperture structure.
Below in conjunction with embodiment and accompanying drawing the present invention is described further, but is not limited to following said content.
Embodiment 1:
(1) earlier with silicone resin and meta particle diameter be the α-Dan Huagui powder of 0.5 μ m according to volume ratio 2:3 batching, add the mixing solutions of absolute ethyl alcohol and toluene, make distributed slurry behind the mixing 12h;
(2) mixed slurry is incubated 12h down at 120 ℃, the gained block is through behind the ball milling, and it is for use to cross 170 mesh sieves;
(3) coated powder of gained and the naphthalene powder of the about 200 μ m of meta particle diameter are carried out uniform mixing, the two mass ratio is 4:1;
(4) with mixed powder at the cold isostatic compaction under 200MPa of compression molding continued under the 50MPa;
(5) adopt ladder-elevating temperature pattern binder removal: 60 ℃/2h, 80 ℃/16h, 100 ℃/4h, 130 ℃/2h;
(6) the gained biscuit is normal pressure-sintered under 1550 ℃, nitrogen atmosphere, temperature rise rate is 5 ℃/min, and soaking time is 4h, promptly obtains a kind of porous SiN ceramic with multistage aperture structure.Its flexural strength is 38.5MPa, and open porosity is 51.25%.
The porous SiN ceramic of present embodiment preparation can be known that by Fig. 2 wherein α-Dan Huagui is a principal phase, beta-silicon nitride and quartzy respectively from the phase transformation of α-Dan Huagui and the cracking of silicone resin; Can know that by Fig. 3 and Fig. 4 its pore diameter range is respectively 10～300 μ m and 0.1～3 μ m.
Embodiment 2:
(1) earlier with silicone resin and meta particle diameter be the α-Dan Huagui powder of 0.5 μ m according to volume ratio 1:2 batching, add the mixing solutions of absolute ethyl alcohol and toluene, make distributed slurry behind the mixing 8h;
(2) mixed slurry is incubated 10h down at 120 ℃, the gained block is through behind the ball milling, and it is for use to cross 180 mesh sieves;
(3) coated powder of gained and the naphthalene powder of the about 200 μ m of meta particle diameter are carried out uniform mixing, the two mass ratio is 3:1;
(4) with mixed powder compression molding under 100MPa;
(5) adopt ladder-elevating temperature pattern binder removal: 60 ℃/2h, 80 ℃/12h, 100 ℃/4h, 120 ℃/2h;
(6) the gained biscuit is normal pressure-sintered under 1500 ℃, nitrogen atmosphere, temperature rise rate is 8 ℃/min, and soaking time is 3h, promptly obtains a kind of porous SiN ceramic with multistage aperture structure.Its flexural strength is 23.5MPa, and open porosity is 52.38%.
The porous SiN ceramic of present embodiment preparation can be known that by Fig. 2 wherein α-Dan Huagui is a principal phase, beta-silicon nitride and quartzy respectively from the phase transformation of α-Dan Huagui and the cracking of silicone resin; Can know that by Fig. 3 and Fig. 4 its pore diameter range is respectively 10～300 μ m and 0.1～3 μ m.
Embodiment 3:
(1) earlier with silicone resin and meta particle diameter be the α-Dan Huagui powder of 1.0 μ m according to volume ratio 3:2 batching, add the mixing solutions of absolute ethyl alcohol and toluene, make distributed slurry behind the mixing 10h;
(2) mixed slurry is incubated 18h down at 100 ℃, the gained block is through behind the ball milling, and it is for use to cross 200 mesh sieves;
(3) with carrying out uniform mixing with the naphthalene powder of the about 150 μ m of meta particle diameter in the coated powder of gained, the two mass ratio is 19:1;
(4) with mixed powder compression molding under 150MPa;
(5) adopt ladder-elevating temperature pattern binder removal: 50 ℃/2h, 85 ℃/16h, 110 ℃/4h, 130 ℃/2h;
(6) the gained biscuit is normal pressure-sintered under 1550 ℃, nitrogen atmosphere, temperature rise rate is 5 ℃/min, and soaking time is 3h, promptly obtains a kind of porous SiN ceramic with multistage aperture structure.Its flexural strength is 87MPa, and open porosity is 39%.
The porous SiN ceramic of present embodiment preparation can be known that by Fig. 2 wherein α-Dan Huagui is a principal phase, beta-silicon nitride and quartzy respectively from the phase transformation of α-Dan Huagui and the cracking of silicone resin; Can know that by Fig. 3 and Fig. 5 its pore diameter range is respectively 10～300 μ m and 0.1～1 μ m.
Embodiment 4:
(1) earlier with silicone resin and meta particle diameter be the α-Dan Huagui powder of 1.0 μ m according to volume ratio 1:1 batching, add the mixing solutions of absolute ethyl alcohol and toluene, make distributed slurry behind the mixing 10h;
(2) mixed slurry is incubated 12h down at 120 ℃, the gained block is through behind the ball milling, and it is for use to sieve;
(3) with carrying out uniform mixing with the naphthalene powder of the about 150 μ m of meta particle diameter in the coated powder of gained, the two mass ratio is 9:1;
(4) with mixed powder compression molding under 150MPa;
(5) adopt ladder-elevating temperature pattern binder removal: 60 ℃/4h, 80 ℃/12h, 100 ℃/6h, 130 ℃/2h;
(6) the gained biscuit is normal pressure-sintered under 1600 ℃, nitrogen atmosphere, temperature rise rate is 4 ℃/min, and soaking time is 2h, promptly obtains a kind of porous SiN ceramic with multistage aperture structure.Its flexural strength is 73MPa, and open porosity is 43.5%.
The porous SiN ceramic of present embodiment preparation can be known that by Fig. 2 wherein α-Dan Huagui is a principal phase, beta-silicon nitride and quartzy respectively from the phase transformation of α-Dan Huagui and the cracking of silicone resin; Can know that by Fig. 6 and Fig. 4 its pore diameter range is respectively 10～300 μ m and 0.1～3 μ m.
Embodiment 5:
(1) earlier with silicone resin and meta particle diameter be the α-Dan Huagui powder of 1.0 μ m according to volume ratio 1:1.85 batching, add the mixing solutions of absolute ethyl alcohol and toluene, make distributed slurry behind the mixing 10h;
(2) mixed slurry is incubated 12h down at 120 ℃, the gained block is through behind the ball milling, and it is for use to cross 170 mesh sieves;
(3) with carrying out uniform mixing with the naphthalene powder of the about 200 μ m of meta particle diameter in the coated powder of gained, the two mass ratio is 1:1;
(4) with mixed powder compression molding under 150MPa;
(5) adopt ladder-elevating temperature pattern binder removal: 60 ℃/2h, 85 ℃/15h, 100 ℃/2h, 130 ℃/2h;
(6) the gained biscuit is normal pressure-sintered under 1500 ℃, nitrogen atmosphere, temperature rise rate is 8 ℃/min, and soaking time is 4h, promptly obtains a kind of porous SiN ceramic with multistage aperture structure.Its flexural strength is 7.8MPa, and open porosity is 71%.
The porous SiN ceramic of present embodiment preparation can be known that by Fig. 2 wherein α-Dan Huagui is a principal phase, beta-silicon nitride and quartzy respectively from the phase transformation of α-Dan Huagui and the cracking of silicone resin; Can know that by Fig. 6 and Fig. 4 its pore diameter range is respectively 10～300 μ m and 0.1～3 μ m.
Embodiment 6:
(1) earlier with silicone resin and meta particle diameter be the α-Dan Huagui powder of 0.5 μ m according to volume ratio 5.7:1 batching, add the mixing solutions of absolute ethyl alcohol and toluene, make distributed slurry behind the mixing 12h;
(2) mixed slurry is incubated 24h down at 120 ℃, the gained block is through behind the ball milling, and it is for use to sieve;
(3) coated powder of gained and the naphthalene powder of the about 100 μ m of meta particle diameter are carried out uniform mixing, the two mass ratio is 19:1;
(4) with mixed powder compression molding under 150MPa;
(5) adopt ladder-elevating temperature pattern binder removal: 60 ℃/2h, 80 ℃/16h, 100 ℃/4h, 130 ℃/2h;
(6) the gained biscuit is normal pressure-sintered under 1550 ℃, nitrogen atmosphere, temperature rise rate is 5 ℃/min, and soaking time is 5h, promptly obtains a kind of porous SiN ceramic with multistage aperture structure.Its flexural strength is 81.7MPa, and open porosity is 25.96%.
The porous SiN ceramic of present embodiment preparation can be known that by Fig. 2 wherein α-Dan Huagui is a principal phase, beta-silicon nitride and quartzy respectively from the phase transformation of α-Dan Huagui and the cracking of silicone resin; Can know that by Fig. 7 and Fig. 8 its pore diameter range is respectively 10～200 μ m and 0.1～2 μ m.
Claims (9)
1. preparation method with high porosity porous SiN ceramic of multistage aperture structure is characterized in that with the silicone resin being sticker and aperture pore-forming material, naphthalene powder for the macropore pore-forming material prepares the method for porous SiN ceramic, and its step comprises:
(1) coats: the α-Dan Huagui powder is mixed with ethanol, obtain the α-Dan Huagui slip; Silicone resin is mixed with toluene, obtain the silicone resin dilute solution; α-Dan Huagui slip and silicone resin dilute solution are mixed, obtain mixed slurry, wherein the volume ratio of α-Dan Huagui and pure silicone resin is 1:9～4:1, and mixing time is 6～24h; The volume(tric)fraction of α-Dan Huagui is 10～80% in the α-Dan Huagui slip, and the silicone resin volume(tric)fraction is 10～50% in the silicone resin dilute solution;
(2) pre-treatment: at 80～120 ℃ of drying 12～24h, the gained solid sieves behind ball milling, obtains coated powder with mixed slurry;
(3) mix: the coated powder and the naphthalene powder of gained are mixed, obtain mixed powder;
(4) moulding: with mixed powder compression molding or mold pressing continued cold isostatic compaction, forming pressure is 10～400 MPa, obtains the moulding sample;
(5) binder removal: employing ladder-elevating temperature pattern at 50～130 ℃ of binder removal 12～24h, obtains biscuit with the moulding sample;
(6) cracking: biscuit is normal pressure-sintered under 1100～1700 ℃, nitrogen atmosphere, and temperature rise rate is 0.5～10 ℃/min, and soaking time is 1～5h, promptly obtains said high porosity porous SiN ceramic with multistage aperture structure.
2. the preparation method of porous SiN ceramic according to claim 1 is characterized in that: described multistage aperture structure is meant that the porous SiN ceramic pore diameter range contains 0.1～500 μ m, is multistage distribution.
3. the preparation method of porous SiN ceramic according to claim 1, it is characterized in that: the porosity of porous SiN ceramic is 25～75%.
4. the preparation method of porous SiN ceramic according to claim 1, it is characterized in that: the volume content of silicone resin is 20～90% in the coated powder.
5. the preparation method of porous SiN ceramic according to claim 1, it is characterized in that: the meta particle diameter of α-Dan Huagui powder is 0.4～5 μ m, the particle diameter of gained coated powder≤100 μ m.
6. the preparation method of porous SiN ceramic according to claim 1 is characterized in that: the meta particle diameter of naphthalene powder≤300 μ m.
7. the preparation method of porous SiN ceramic according to claim 1, it is characterized in that: in the described mixed powder, the mass ratio of coated powder and naphthalene powder is 19:1～1:1.
8. the preparation method of porous SiN ceramic according to claim 1, it is characterized in that: compression molding pressure is 10～150MPa; Or mold pressing continued cold isostatic compaction, forming pressure is 100～400MPa.
9. the preparation method of porous SiN ceramic according to claim 1 is characterized in that: described employing ladder-elevating temperature pattern, i.e. 50～70 ℃ of insulation 1～2h; Be warming up to 70～90 ℃ of insulation 8～16h; Be warming up to 90～110 ℃ of insulation 2～8h; Be warming up to 110～130 ℃ of insulation 1～4h at last.
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| CN117229067A (en) * | 2023-11-14 | 2023-12-15 | 中南大学 | Method for preparing silicon nitride ceramics by low-pressure nitridation-embedding |
| CN117229067B (en) * | 2023-11-14 | 2024-02-23 | 中南大学 | Method for preparing silicon nitride ceramics by low-pressure nitridation-embedding |
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