CN1803717A - Method for preparing SiAlON ceramic powder by sea mud and sand - Google Patents
Method for preparing SiAlON ceramic powder by sea mud and sand Download PDFInfo
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- CN1803717A CN1803717A CN 200610011256 CN200610011256A CN1803717A CN 1803717 A CN1803717 A CN 1803717A CN 200610011256 CN200610011256 CN 200610011256 CN 200610011256 A CN200610011256 A CN 200610011256A CN 1803717 A CN1803717 A CN 1803717A
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Abstract
The provided preparation method for SiAlON ceramic powder with sea silt comprises: selecting material to dry, crush and mix with carbon and Al2O3; ball grinding the mixture in water with added NaH2PO4 and SCMC; slip casting the obtained slurry in gypsum mold to prepare blank; drying and sintering the blank in Si3N4 powder and nitrogen atmosphere; finally, removing the residual carbon to obtain the final product with principal crystalline phase as 75-95wt% O'-SiAlON, paracrystalline phase as 3-20% SiC. This invention has wide application.
Description
Technical field
The invention belongs to technical field of ceramic material, a kind of method of utilizing sea mud and sand to prepare the SiAlON ceramic powder particularly is provided, the product of preparation has higher degree.
Background technology
SiAlON is a kind of structural ceramics of premium properties, as very high normal temperature and hot strength, excellent normal temperature and stability at elevated temperature, very strong wear resistance, good thermostability is with a wide range of applications at industrial circles such as metallurgy, chemical industry, electric power, the energy.O '-SiAlON is a kind of important SiAlON family material, has splendid antioxidant property and lower thermal expansivity, is a kind of up-and-coming engineering ceramics.
Employing solid reaction process and combustion synthesis method can prepare the O '-SiAlON material of high purity, excellent property, but because the restriction of raw material and technology, cost is too expensive, has limited its large-scale application.And utilize the carbothermal reduction-nitridation method can prepare O '-SiAlON at lower cost, but be difficult to prepare high purity, high performance O '-SiAlON material.
(the patent No.: mention a kind of river sand that utilizes 00105941.6) and be main raw material of " utilizing river sand to prepare the way of Sailong and silicon carbide combined ceramic powder " in patent of invention, the carbothermal reduction-nitridation method is synthesized the Sailong and silicon carbide combined ceramic powder, but the forming technique that adopts in this invention is dry-pressing formed, be different from the injection forming among the present invention, and principal crystalline phase is SiC (mass percent is 50-80%) in the end article.
Also repeatedly mention in some academic papers and utilize the carbothermal reduction-nitridation legal system to be equipped with O '-SiAlON and composite material powder thereof, the present invention possesses several characteristics and innovative point simultaneously: adopt the slip-casting shaping process molding blank; Main raw material is the extremely abundant sea sand resources of reserves; O ' in the gained powder-SiAlON content height.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing sea mud and sand to prepare the SiAlON ceramic powder, can obtain the having higher degree SiAlON ceramic powder of (mass percent is 75-95%).
The present invention is main raw material with the sea mud and sand, is equipped with O '-SiAlON powder by the carbothermal reduction-nitridation legal system, has used the uniform high-performance base substrate of slip-casting shaping process prepared composition.In preparation process by control ratio of components, sintering temperature, sintering time, nitrogen flow and bury processing parameter such as vermicelli spare, can obtain the having higher degree SiAlON ceramic powder of (mass percent is 75-95%).Processing step is:
1. related sea mud and sand (abbreviation sea sand) principal crystalline phase SiO among the present invention
2(its mass percent is 70-90%) and Al
2O
3(mass percent is 3-15%), all the other compositions comprise: the oxide compound of K, Fe, Mg, Ca element.
2. with the broken sieve of pulverizing 0.074mm of sea sand raw material, with sea sand, Al
2O
3, carbon (graphite or carbon black) is according to 100: (0-10): mass percent (20-35) is mixed.
3. add SODIUM PHOSPHATE, MONOBASIC solvent that mass percent is 0.2-2% and the Xylo-Mucine of 0.05-0.5% in compound respectively, adding water, to form solid volume content be the slurry of 35-55%, under the normal temperature ball milling 6-20 hour, forms stable dispersion suspension.
4. slurry is poured into a mould after the demoulding under 50-150 ℃ of temperature dry 10-40 hour in gypsum mold.
5. base substrate after the drying is put into tube furnace, adopt Si
3N
4Bury powder, feed the nitrogen gas stream of 0.2-2.0 liter/minute flow, to 1400-1550 ℃, be incubated 4-10 hour with 5-15 ℃/minute temperature rise rate elevated temperature; Naturally cool to 600 ℃ and stop logical nitrogen, continue to be cooled to 50-200 ℃ and take out goods behind the sintering.
6. goods behind the sintering are heated to 700-800 ℃ in oxidizing atmosphere, are incubated 1.5-2.5 hour, remove the residue carbon elements in the sample piece; Obtaining principal crystalline phase is that O '-SiAlON, paracrystalline phase are the end article of SiC, and the SiAlON mass percent is 75-95% in the goods, and the SiC mass percent is 3-20%, and all the other are the impurity phase.
The invention has the advantages that: obtain the having higher degree SiAlON ceramic powder of (mass percent is 75-95%).Can be widely used in industrial circles such as metallurgy, chemical industry, electric power, the energy.By the Technology of lower cost, prepared the SiAlON ceramic powder of excellent property, make natural resources obtain rationally utilizing fully.
Description of drawings
Fig. 1 is the XRD figure spectrum of gained powder in the embodiment of the invention 1.
Fig. 2 is the XRD figure spectrum of gained powder in the embodiment of the invention 2.
Embodiment
To enumerate some embodiments of the invention below, in the following example, used silt is taken from Xiamen sea area sandy beach, the East Sea.It consists of:
| Composition | SiO 2 | Al 2O 3 | K 2O | Fe 2O 3 | Surplus |
| Mass percent (%) | 87.8 | 5.0 | 3.5 | 2.6 | 1.1 |
Embodiment 1
The Xiamen sea sand was dried 10 hours under 100 ℃ of temperature, utilize the electromagnetism pulverizer that it was crushed to the sieve of 0.074mm.
With silt, Al
2O
3, graphite mixes according to 100: 2: 25 mass percent.
Adding mass percent is the Xylo-Mucine of 0.4%SL type organic solvent and 0.1%, and adding water, to form solid volume content be 50% slurry.
Ball milling is 14 hours under the normal temperature, forms stable dispersion suspension.
Slurry is poured into a mould in gypsum mold.
Gained base substrate under 80 ℃ of temperature dry 20 hours.
Base substrate after the drying is put into tube furnace, adopt Si
3N
4Bury powder, feed the nitrogen gas stream of 0.5 liter of/minute flow,, be incubated 4 hours with 10 ℃/minute temperature rise rate elevated temperatures to 1450 ℃.
Naturally cooling stops logical nitrogen to 600 ℃, takes out sample piece behind the sintering to 100 ℃.
Sample is heated to 700 ℃ in oxidizing atmosphere, is incubated 2 hours, remove the residue carbon elements in the sample piece.
Principal crystalline phase is Si in the end article that obtains
1.6Al
0.4O
1.4N
1.6, contain part of SiC and trace impurity phase.
Embodiment 2:
The Xiamen sea sand was dried 10 hours under 100 ℃ of temperature, utilize the electromagnetism pulverizer that it was pulverized the sieve of 0.074mm.
With sand, Al
2O
3, carbon black mixes according to 100: 2: 25 mass percent.
Adding mass percent is the Xylo-Mucine of 0.4%SL type organic solvent and 0.1%, and adding water, to form solid volume content be 50% slurry.
Ball milling is 14 hours under the normal temperature, forms stable dispersion suspension.
Slurry is poured into a mould in gypsum mold.
Gained base substrate under 80 ℃ of temperature dry 20 hours.
Base substrate after the drying is put into tube furnace, adopt Si
3N
4Bury powder, feed the nitrogen gas stream of 0.5 liter of/minute flow,, be incubated 4 hours with 10 ℃/minute temperature rise rate elevated temperatures to 1450 ℃.
Naturally cooling stops logical nitrogen to 600 ℃, takes out sample piece behind the sintering to 100 ℃.
Sample is heated to 700 ℃ in oxidizing atmosphere, is incubated 2 hours, remove the residue carbon elements in the sample piece.
Principal crystalline phase is Si in the end article that obtains
1.6Al
0.4O
1.4N
1.6, contain part of SiC and trace impurity phase.
Embodiment 3:
The Xiamen sea sand was dried 10 hours under 100 ℃ of temperature, utilize the electromagnetism pulverizer that it was crushed to the sieve of 0.074mm.
With sand, Al
2O
3, graphite mixes according to 100: 4: 30 mass percent.
Adding mass percent is the Xylo-Mucine of 1.2%SL type organic solvent and 0.2%, and adding water, to form solid volume content be 45% slurry.
Ball milling is 12 hours under the normal temperature, forms stable dispersion suspension.
Slurry is poured into a mould in gypsum mold.
Gained base substrate under 80 ℃ of temperature dry 20 hours.
Base substrate after the drying is put into tube furnace, adopt Si
3N
4Bury powder, feed the nitrogen gas stream of 0.3 liter of/minute flow,, be incubated 6 hours with 10 ℃/minute temperature rise rate elevated temperatures to 1480 ℃.
Naturally cooling stops logical nitrogen to 600 ℃, takes out sample piece behind the sintering to 100 ℃.
Sample is heated to 700 ℃ in oxidizing atmosphere, is incubated 2 hours, remove the residue carbon elements in the sample piece.
Principal crystalline phase is Si in the end article that obtains
1.6Al
0.4O
1.4N
1.6, contain part of SiC and trace impurity phase.
Embodiment 4:
The Xiamen sea sand was dried 10 hours under 100 ℃ of temperature, utilize the electromagnetism pulverizer that it was crushed to the sieve of 0.074mm.
With sand, Al
2O
3, graphite mixes according to 100: 4: 30 mass percent.
Adding mass percent is the Xylo-Mucine of 1.0%SL type organic solvent and 0.25%, and adding water, to form solid volume content be 45% slurry.
Ball milling is 16 hours under the normal temperature, forms stable dispersion suspension.
Slurry is poured into a mould in gypsum mold.
Gained base substrate under 80 ℃ of temperature dry 20 hours.
Base substrate after the drying is put into tube furnace, adopt Si
3N
4Bury powder, feed the nitrogen gas stream of 0.6 liter of/minute flow,, be incubated 4 hours with 10 ℃/minute temperature rise rate elevated temperatures to 1420 ℃.
Naturally cooling stops logical nitrogen to 600 ℃, takes out sample piece behind the sintering to 100 ℃.
Sample is heated to 700 ℃ in oxidizing atmosphere, is incubated 2 hours, remove the residue carbon elements in the sample piece.
Principal crystalline phase is Si in the end article that obtains
1.6Al
0.4O
1.4N
1.6, contain part of SiC and trace impurity phase.
Claims (3)
1, a kind of method of utilizing sea mud and sand to prepare the SiAlON ceramic powder, it is characterized in that: processing step is:
A, with the broken 0.074mm sieve that was crushed to of sea sand raw material, with sea sand, Al
2O
3, carbon is according to 100: (0-10): mass percent (20-35) is mixed;
B, to add mass percent in compound respectively be the SODIUM PHOSPHATE, MONOBASIC solvent of 0.2-2% and the Xylo-Mucine solvent of 0.05-0.5%, adding water formation solid volume content is the slurry of 35-55%, under the normal temperature ball milling 6-20 hour, form stable dispersion suspension;
C, slurry is poured into a mould after the demoulding under 50-150 ℃ of temperature dry 10-40 hour in gypsum mold;
D, base substrate after the drying is put into tube furnace, adopt Si
3N
4Bury powder, feed the nitrogen gas stream of 0.2-2.0 liter/minute flow, to 1400-1550 ℃, be incubated 4-10 hour with 5-15 ℃/minute temperature rise rate elevated temperature; Naturally cool to 600 ℃ and stop logical nitrogen, continue to be cooled to 50-200 ℃ and take out goods behind the sintering;
E, goods behind the sintering are heated to 700-800 ℃ in oxidizing atmosphere, are incubated 1.5-25 hour, remove the residue carbon elements in the sample piece; Obtaining principal crystalline phase is that O '-SiAlON, paracrystalline phase are the end article of SiC, and the SiAlON mass percent is 75-95% in the goods, and the SiC mass percent is 3-20%, and all the other are the impurity phase.
2, in accordance with the method for claim 1, it is characterized in that: the sea sand principal crystalline phase is SiO
2And Al
2O
3, SiO wherein
2Mass percent be 70-90%, Al
2O
3Mass percent be 3-15%, all the other compositions comprise: the oxide compound of K, Fe, Mg, Ca element.
3, in accordance with the method for claim 1, it is characterized in that: described carbon is graphite or carbon black.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610011256 CN1803717A (en) | 2006-01-23 | 2006-01-23 | Method for preparing SiAlON ceramic powder by sea mud and sand |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610011256 CN1803717A (en) | 2006-01-23 | 2006-01-23 | Method for preparing SiAlON ceramic powder by sea mud and sand |
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|---|---|
| CN1803717A true CN1803717A (en) | 2006-07-19 |
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ID=36865896
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|---|---|---|---|
| CN 200610011256 Pending CN1803717A (en) | 2006-01-23 | 2006-01-23 | Method for preparing SiAlON ceramic powder by sea mud and sand |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100418924C (en) * | 2007-04-27 | 2008-09-17 | 北京科技大学 | Method for preparing Ca-alpha-SiAlON material using iron selection tailings |
| CN115504791A (en) * | 2022-08-12 | 2022-12-23 | 河南好运祥耐材有限公司 | O' -SiAlON-SiC prefabricated part with high oxidation resistance and preparation method thereof |
-
2006
- 2006-01-23 CN CN 200610011256 patent/CN1803717A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100418924C (en) * | 2007-04-27 | 2008-09-17 | 北京科技大学 | Method for preparing Ca-alpha-SiAlON material using iron selection tailings |
| CN115504791A (en) * | 2022-08-12 | 2022-12-23 | 河南好运祥耐材有限公司 | O' -SiAlON-SiC prefabricated part with high oxidation resistance and preparation method thereof |
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