CN106977185A - A kind of aluminium oxide ceramics and preparation method thereof - Google Patents
A kind of aluminium oxide ceramics and preparation method thereof Download PDFInfo
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- CN106977185A CN106977185A CN201710386104.4A CN201710386104A CN106977185A CN 106977185 A CN106977185 A CN 106977185A CN 201710386104 A CN201710386104 A CN 201710386104A CN 106977185 A CN106977185 A CN 106977185A
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Abstract
The invention discloses a kind of aluminium oxide ceramics and preparation method thereof.First binding agent is wrapped in inorganic powder surface by the aluminium oxide ceramics using silane coupler, strengthens the mobility and uniformity between inorganic particle, in scouring processes, and binding agent can be equably from internal breakup, diffusion without forming or forming hole and crackle less；Second aluminium hydroxide, silane coupler and binding agent can be decomposed, while producing aluminum oxide and silica, are filled with issuable hole and crackle, added product compactness；Three the adhesion between aluminum oxide and magnesia can strengthen under the induction of magnesium aluminate spinel, under the collective effect of above-mentioned three functions, improve the hardness and intensity of aluminium oxide ceramics.While its hardness and intensity is improved, cooperated by magnesium aluminate spinel and magnesia, it is common to suppress alumina grain growth, intercrystalline pore is eliminated, defect is reduced, stress concentration point is reduced, improves its toughness.
Description
Technical field
The invention belongs to field of ceramic preparation technology, and in particular to a kind of aluminium oxide ceramics and preparation method thereof, especially relate to
And a kind of Aqueous injection formed alumina ceramics and preparation method thereof.
Background technology
The features such as aluminium oxide ceramics has high temperature resistant, wear-resistant, electric insulation, anti-oxidant, corrosion-resistant and high mechanical strength, on
Stating outstanding physicochemical property makes it be had a wide range of applications demand in various fields such as national defence, building, chemical industry and smeltings.Many institute's weeks
Know, on microcosmic, alumina ceramic material is the material that a kind of covalent bond and ionic bond are combined into, because combining the direction of valence link
Property causes the material to have the shortcomings that high fragility and low toughness, causes it to be broken under extremely low strain value, the big day of one's doom
The extensive use of aluminium oxide ceramics is made.
When in face of above mentioned problem, researcher has invented many method for toughening, wherein common are phase toughness, whisker
And particle toughening, fiber toughening, nano wire or nanotube toughening etc..But phase transformation, whisker and particle toughening effect are not special
Substantially；The opertions engineering of fiber toughening is complex, while the consistency of product is poor；Nano wire or nanotube toughening are typically adopted
With carbon nanocoils or nanotube, at high temperature, it easily reacts to reduce toughening effect with matrix material.In order to obtain
Good toughening effect, researcher attempts to use two or more method for toughening, such as, Chinese patent literature
CN101948325A discloses a kind of synergistic toughening alumina ceramic and preparation method thereof.The technology employs phase toughness and crystalline substance
Palpus toughening, improves the toughness of aluminium oxide ceramics.
The compound for the silicon that above-mentioned technology is used during aluminium oxide ceramics is prepared, the compound of zirconium, the chemical combination of yttrium
Thing is intended to be dissolved in solvent, and this large amount of solvent that just volatilized in follow-up drying process, these solvent flashings easily cause aluminum oxide to be made pottery
Porcelain ftractures, and causes the aluminium oxide ceramics porosity high, it is difficult to form fine and close structure；Furthermore, in dumping, binding agent equally can be big
Amount volatilization, forms space in ceramics.Above-mentioned two situations can have a strong impact on the hardness and intensity of aluminium oxide ceramics.
The content of the invention
Therefore, existing aluminium oxide ceramics to be solved by this invention is easily caused aluminium oxide ceramics while its toughness is improved
Hardness and the defect that declines of intensity, and then provide a kind of hardness and intensity is high and the low oxygen of good toughness, the not easy to crack, porosity
Change aluminium ceramics and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
Aluminium oxide ceramics provided by the present invention, includes the raw material of following parts by weight：
Further, 0.1-0.2 parts of rare earth oxide is included.
Further, the rare earth oxide is at least one of cerium oxide, lanthana, yittrium oxide or ytterbium oxide.
Further, the particle diameter of the aluminum oxide is that 20-50nm, purity are 99.99%；
The binding agent is at least one of paraffin, stearic acid, polyethylene and polypropylene.
In addition, present invention also offers the preparation method of above-mentioned aluminium oxide ceramics, comprising the following steps：
1) aluminum oxide, aluminium hydroxide, magnesia, kaolin, magnesium aluminate spinel and silane coupler are mixed in proportion and ground
Mill, obtains compound；
2) after adhesive heating, then the compound is added thereto and mixed；
3) to step 2) processing after compound be molded, obtain article shaped；
4) carry out degumming successively to the article shaped, burn till, obtain aluminium oxide ceramics.
Further, step 2) in, the temperature of the heating is 100-180 DEG C.
Further, step 3) in, it is described to be shaped to injection moulding.
Further, the injection molding temperature is 150-190 DEG C, and briquetting pressure is 2-4Mpa, and molding time is 5-
10s。
Further, step 4) in, the temperature of the degumming is 600-700 DEG C；
The temperature burnt till is 1200-1500 DEG C.
Further, the temperature control burnt till is as follows：
(1) with 4-5h from room temperature to 600-700 DEG C；
(2) it is incubated 1-2h at 600-700 DEG C；
(3) it is warming up to 1200-1500 DEG C from 600-700 DEG C with 7-8h；
(4) it is incubated 15-20h at 1200-1500 DEG C.
In the present invention, the composition of magnesium aluminate spinel is MgAl2O4, silane coupler is specially KH550.
Compared with prior art, the present invention has the advantages that：
(1) aluminium oxide ceramics that the embodiment of the present invention is provided, it is brilliant using aluminium hydroxide, silane coupler and magnalium point
Stone, and used cooperatively with other raw materials, binding agent is tightly first wrapped in inorganic powder surface using silane coupler, makes nothing
Between machine powder uniformly separate, enhancing inorganic particle between mobility and uniformity, in scouring processes, binding agent can equably from
Internal breakup, diffusion are without forming or forming hole and crackle less；Second in subsequent forming, degumming and sintering process, hydrogen-oxygen
Changing aluminium, silane coupler and binding agent can decompose, while produce aluminum oxide and silica, be filled with issuable hole and
Crackle, adds product compactness；Three under the induction of magnesium aluminate spinel, the adhesion between aluminum oxide and magnesia can increase
By force, under the collective effect of above-mentioned three functions, the hardness and intensity of aluminium oxide ceramics are improved.Improving its hardness and intensity
While, cooperated by magnesium aluminate spinel and magnesia, it is common to suppress alumina grain growth, intercrystalline pore is eliminated,
Defect is reduced, stress concentration point is reduced, improves its toughness.
(2) aluminium oxide ceramics that the embodiment of the present invention is provided, using rare earth oxide, itself and magnesium aluminate spinel, oxidation
Magnesium cooperates, and improves the corresponding effect of magnesium aluminate spinel and magnesia, meanwhile, make alumina grain size homogeneous, disperse
Uniformly, and then disperse stress, improve toughness.
(3) preparation method for the aluminium oxide ceramics that the embodiment of the present invention is provided, first by aluminum oxide, aluminium hydroxide, oxidation
Magnesium, kaolin, magnesium aluminate spinel and silane coupler mixed grinding in proportion, make each stock dispersion uniform, it is to avoid segregation occur
Phenomenon；In the binding agent for adding mixture into melting again, binding agent is tightly wrapped in inorganic powder body surface using silane coupler
Face, makes uniformly to separate between inorganic particle, mobility and uniformity between enhancing inorganic particle, in scouring processes, binding agent energy
Equably from internal breakup, diffusion without being formed or forming hole and crackle less；Finally, it is molded, degumming and is burnt till, hydrogen-oxygen
Changing aluminium, silane coupler and binding agent can decompose, while produce aluminum oxide and silica, be filled with issuable hole and
Crackle, adds product compactness；Simultaneously under the induction of magnesium aluminate spinel, the adhesion between aluminum oxide and magnesia can increase
By force, under the collective effect of above-mentioned three functions, the hardness and intensity of aluminium oxide ceramics are improved.Improving its hardness and intensity
While, cooperated by magnesium aluminate spinel and magnesia, it is common to suppress alumina grain growth, intercrystalline pore is eliminated,
Defect is reduced, stress concentration point is reduced, improves its toughness.
Embodiment
In order to which the object, technical solutions and advantages of the present invention are better described, below in conjunction with specific embodiment to this hair
It is bright to be described further.The present invention can be embodied in many different forms, and should not be construed as limited to set forth herein
Embodiment.Opposite there is provided these embodiments so that the disclosure will be thorough and complete, and the design of the present invention will be filled
Divide and convey to those skilled in the art, the present invention will only be defined by the appended claims.
Embodiment 1
A kind of aluminium oxide ceramics is present embodiments provided, is made up of the raw material of following parts by weight：
90g particle diameter is 40nm, the aluminum oxide that purity is 99.99%, 17g aluminium hydroxide, 5.5g magnesia, 7.5g
Silane coupler-KH550,3.5g binding agent-stearic acid, 6.5g kaolin and 5g magnesium aluminate spinel；
The preparation method of above-mentioned aluminium oxide ceramics, comprises the following steps：
1) aluminum oxide, aluminium hydroxide, magnesia, kaolin, magnesium aluminate spinel and silane coupler are mixed in proportion and ground
It is milled to particle diameter and is not more than 1 μm, obtains compound；
2) adhesive heating is added thereto and mixed to 140 DEG C, then by the compound；
3) to step 2) processing after compound carry out injection moulding, article shaped is obtained, wherein injection molding temperature is
155 DEG C, briquetting pressure is 3Mpa, and molding time is 8s；
4) article shaped is burnt till 18h at 1300 DEG C, obtains aluminium oxide ceramics in degumming at 650 DEG C.
Embodiment 2
A kind of aluminium oxide ceramics is present embodiments provided, is made up of the raw material of following parts by weight：
85g particle diameter is 20nm, the aluminum oxide that purity is 99.99%, 20g aluminium hydroxide, 5g magnesia, 8g silicon
Alkane coupling agent-KH550,3g binding agent-paraffin, 7g kaolin and 4g magnesium aluminate spinel；
The preparation method of above-mentioned aluminium oxide ceramics, comprises the following steps：
1) aluminum oxide, aluminium hydroxide, magnesia, kaolin, magnesium aluminate spinel and silane coupler are mixed in proportion and ground
It is milled to particle diameter and is not more than 1 μm, obtains compound；
2) adhesive heating is added thereto and mixed to 100 DEG C, then by the compound；
3) to step 2) processing after compound carry out injection moulding, article shaped is obtained, wherein injection molding temperature is
150 DEG C, briquetting pressure is 4Mpa, and molding time is 5s；
4) article shaped is burnt till 15h at 1500 DEG C, obtains aluminium oxide ceramics in degumming at 600 DEG C.
Embodiment 3
A kind of aluminium oxide ceramics is present embodiments provided, is made up of the raw material of following parts by weight：
95g particle diameter is 50nm, the aluminum oxide that purity is 99.99%, 15g aluminium hydroxide, 6g magnesia, 7g silicon
Alkane coupling agent-KH550,4g binding agent-polypropylene, 6g kaolin and 6g magnesium aluminate spinel；
The preparation method of above-mentioned aluminium oxide ceramics, comprises the following steps：
1) aluminum oxide, aluminium hydroxide, magnesia, kaolin, magnesium aluminate spinel and silane coupler are mixed in proportion and ground
It is milled to particle diameter and is not more than 1 μm, obtains compound；
2) adhesive heating is added thereto and mixed to 180 DEG C, then by the compound；
3) to step 2) processing after compound carry out injection moulding, article shaped is obtained, wherein injection molding temperature is
190 DEG C, briquetting pressure is 2Mpa, and molding time is 10s；
4) article shaped is burnt till 20h at 1200 DEG C, obtains aluminium oxide ceramics in degumming at 700 DEG C.
Embodiment 4
A kind of aluminium oxide ceramics is present embodiments provided, is made up of the raw material of following parts by weight：
90g particle diameter is 40nm, the aluminum oxide that purity is 99.99%, 17g aluminium hydroxide, 5.5g magnesia, 7.5g
Silane coupler-KH550,3.5g binding agent-stearic acid, 6.5g kaolin, 5g magnesium aluminate spinel and 0.1g oxygen
Change lanthanum；
The preparation method of above-mentioned aluminium oxide ceramics, comprises the following steps：
1) by aluminum oxide, aluminium hydroxide, magnesia, kaolin, magnesium aluminate spinel, silane coupler and lanthana in proportion
Mixed grinding to particle diameter is not more than 1 μm, obtains compound；
2) adhesive heating is added thereto and mixed to 140 DEG C, then by the compound；
3) to step 2) processing after compound carry out injection moulding, article shaped is obtained, wherein injection molding temperature is
155 DEG C, briquetting pressure is 3Mpa, and molding time is 8s；
4) article shaped is burnt till 18h at 1300 DEG C, obtains aluminium oxide ceramics in degumming at 650 DEG C.
Embodiment 5
A kind of aluminium oxide ceramics is present embodiments provided, is made up of the raw material of following parts by weight：
85g particle diameter is 20nm, the aluminum oxide that purity is 99.99%, 20g aluminium hydroxide, 5g magnesia, 8g silicon
Alkane coupling agent-KH550,3g binding agent-paraffin, 7g kaolin, 4g magnesium aluminate spinel and 0.2g cerium oxide；
The preparation method of above-mentioned aluminium oxide ceramics, comprises the following steps：
1) by aluminum oxide, aluminium hydroxide, magnesia, kaolin, magnesium aluminate spinel, silane coupler and cerium oxide in proportion
Mixed grinding to particle diameter is not more than 1 μm, obtains compound；
2) adhesive heating is added thereto and mixed to 100 DEG C, then by the compound；
3) to step 2) processing after compound carry out injection moulding, article shaped is obtained, wherein injection molding temperature is
150 DEG C, briquetting pressure is 4Mpa, and molding time is 5s；
4) article shaped is burnt till 15h at 1500 DEG C, obtains aluminium oxide ceramics in degumming at 600 DEG C.
Embodiment 6
A kind of aluminium oxide ceramics is present embodiments provided, is made up of the raw material of following parts by weight：
95g particle diameter is 50nm, the aluminum oxide that purity is 99.99%, 15g aluminium hydroxide, 6g magnesia, 7g silicon
Alkane coupling agent-KH550,4g binding agent-polypropylene, 6g kaolin and 6g magnesium aluminate spinel；
The preparation method of above-mentioned aluminium oxide ceramics, comprises the following steps：
1) aluminum oxide, aluminium hydroxide, magnesia, kaolin, magnesium aluminate spinel and silane coupler are mixed in proportion and ground
It is milled to particle diameter and is not more than 1 μm, obtains compound；
2) adhesive heating is added thereto and mixed to 180 DEG C, then by the compound；
3) to step 2) processing after compound carry out injection moulding, article shaped is obtained, wherein injection molding temperature is
190 DEG C, briquetting pressure is 2Mpa, and molding time is 10s；
4) by the article shaped in degumming at 700 DEG C；After cooling, then with 4h from room temperature to 600 DEG C, and at 600 DEG C
Lower insulation 2h；Then, 1200 DEG C are warming up to from 600 DEG C with 8h, and in being incubated 20h at 1200 DEG C, obtain aluminium oxide ceramics.
Embodiment 7
A kind of aluminium oxide ceramics is present embodiments provided, is made up of the raw material of following parts by weight：
90g particle diameter is 40nm, the aluminum oxide that purity is 99.99%, 17g aluminium hydroxide, 5.5g magnesia, 7.5g
Silane coupler-KH550,3.5g binding agent (wherein, paraffin 0.5g, stearic acid 1g, polyethylene 2g), 6.5g kaolin
With 5g magnesium aluminate spinel；
The preparation method of above-mentioned aluminium oxide ceramics, comprises the following steps：
1) aluminum oxide, aluminium hydroxide, magnesia, kaolin, magnesium aluminate spinel and silane coupler are mixed in proportion and ground
It is milled to particle diameter and is not more than 1 μm, obtains compound；
2) adhesive heating is added thereto and mixed to 140 DEG C, then by the compound；
3) to step 2) processing after compound carry out injection moulding, article shaped is obtained, wherein injection molding temperature is
155 DEG C, briquetting pressure is 3Mpa, and molding time is 8s；
4) article shaped is burnt till 18h at 1300 DEG C, obtains aluminium oxide ceramics in degumming at 650 DEG C.
Comparative example 1
This comparative example provides a kind of aluminium oxide ceramics, is made up of the raw material of following parts by weight：
90g particle diameter is 40nm, the aluminum oxide that purity is 99.99%, 17g aluminium hydroxide, 5.5g magnesia, 3.5g
Binding agent-stearic acid, 6.5g kaolin and 5g magnesium aluminate spinel；
The preparation method of above-mentioned aluminium oxide ceramics, comprises the following steps：
1) by aluminum oxide, aluminium hydroxide, magnesia, kaolin and magnesium aluminate spinel, mixed grinding is little to particle diameter in proportion
In 1 μm, compound is obtained；
2) adhesive heating is added thereto and mixed to 140 DEG C, then by the compound；
3) to step 2) processing after compound carry out injection moulding, article shaped is obtained, wherein injection molding temperature is
155 DEG C, briquetting pressure is 3Mpa, and molding time is 8s；
4) article shaped is burnt till 18h at 1300 DEG C, obtains aluminium oxide ceramics in degumming at 650 DEG C.
Comparative example 2
This comparative example provides a kind of aluminium oxide ceramics, is made up of the raw material of following parts by weight：
90g particle diameter is 40nm, the aluminum oxide that purity is 99.99%, 17g aluminium hydroxide, 5.5g magnesia, 7.5g
Silane coupler-KH550,3.5g binding agent-stearic acid and 6.5g kaolin；
The preparation method of above-mentioned aluminium oxide ceramics, comprises the following steps：
1) by aluminum oxide, aluminium hydroxide, magnesia, kaolin and silane coupler, mixed grinding is little to particle diameter in proportion
In 1 μm, compound is obtained；
2) adhesive heating is added thereto and mixed to 140 DEG C, then by the compound；
3) to step 2) processing after compound carry out injection moulding, article shaped is obtained, wherein injection molding temperature is
155 DEG C, briquetting pressure is 3Mpa, and molding time is 8s；
4) article shaped is burnt till 18h at 1300 DEG C, obtains aluminium oxide ceramics in degumming at 650 DEG C.
Comparative example 3
This comparative example provides a kind of aluminium oxide ceramics, is made up of the raw material of following parts by weight：
90g particle diameter be 40nm, the aluminum oxide that purity is 99.99%, 5.5g magnesia, 7.5g silane coupler-
The magnesium aluminate spinel of KH550,3.5g binding agent-stearic acid, 6.5g kaolin and 5g；
The preparation method of above-mentioned aluminium oxide ceramics, comprises the following steps：
1) by aluminum oxide, magnesia, kaolin, magnesium aluminate spinel and silane coupler in proportion mixed grinding to particle diameter not
More than 1 μm, compound is obtained；
2) adhesive heating is added thereto and mixed to 140 DEG C, then by the compound；
3) to step 2) processing after compound carry out injection moulding, article shaped is obtained, wherein injection molding temperature is
155 DEG C, briquetting pressure is 3Mpa, and molding time is 8s；
4) article shaped is burnt till 18h at 1300 DEG C, obtains aluminium oxide ceramics in degumming at 650 DEG C.
Test example 1
Hardness, intensity and toughness to the aluminium oxide ceramics obtained by the various embodiments described above and comparative example are tested, phase
The test result answered is as shown in table 1 below：
Hardness, intensity and the toughness data of the aluminium oxide ceramics of table 1
| Rockwell hardness/HRA | Compression strength/MPa | Fracture toughness/MPam1/2 | Bending strength/MPa | |
| Embodiment 1 | 90 | 890 | 9.8 | 900 |
| Embodiment 2 | 88 | 875 | 9.4 | 898 |
| Embodiment 3 | 87 | 870 | 9.4 | 898 |
| Embodiment 4 | 95 | 1100 | 11 | 905 |
| Embodiment 5 | 94 | 1000 | 11.5 | 910 |
| Embodiment 6 | 89 | 880 | 9.5 | 900 |
| Embodiment 7 | 93 | 900 | 10 | 905 |
| Comparative example 1 | 75 | 530 | 5.5 | 400 |
| Comparative example 2 | 60 | 500 | 4.8 | 290 |
| Comparative example 3 | 77 | 550 | 5.4 | 410 |
It can be learnt from table 1：Many obtained aluminium oxide ceramics of the invention are respectively provided with excellent in terms of hardness, intensity and toughness
Characteristic, reason is：First binding agent is tightly wrapped in inorganic powder surface using silane coupler, made between inorganic particle
It is even separated, enhancing inorganic particle between mobility and uniformity, in scouring processes, binding agent can equably from internal breakup,
Diffusion is without forming or forming hole and crackle less；Second in subsequent forming, degumming and sintering process, aluminium hydroxide, silane
Coupling agent and binding agent can be decomposed, while producing aluminum oxide and silica, be filled with issuable hole and crackle, be increased
Product compactness；Three under the induction of magnesium aluminate spinel, the adhesion between aluminum oxide and magnesia can strengthen, above-mentioned three
Then under the collective effect of function, the hardness and intensity of aluminium oxide ceramics are improved.While its hardness and intensity is improved, pass through
Magnesium aluminate spinel and magnesia cooperate, common to suppress alumina grain growth, eliminate intercrystalline pore, reduce defect, drop
Stress concentration point, improves its toughness.
Test example 2
Porosity to the aluminium oxide ceramics obtained by the various embodiments described above and comparative example is tested, corresponding test knot
It is really as shown in table 2 below：
The porosity data of the aluminium oxide ceramics of table 2
| Porosity/% | |
| Embodiment 1 | 0.10 |
| Embodiment 2 | 0.11 |
| Embodiment 3 | 0.11 |
| Embodiment 4 | 0.08 |
| Embodiment 5 | 0.09 |
| Embodiment 6 | 0.1 |
| Embodiment 7 | 0.12 |
| Comparative example 1 | 10 |
| Comparative example 2 | 8 |
| Comparative example 3 | 9 |
It can be learnt from table 2：The porosity of aluminium oxide ceramics produced by the present invention is low, compact structure, and then with excellent
Hardness and intensity.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1. a kind of aluminium oxide ceramics, includes the raw material of following parts by weight：
2. aluminium oxide ceramics according to claim 1, it is characterised in that also include 0.1-0.2 parts of rare earth oxide.
3. aluminium oxide ceramics according to claim 2, it is characterised in that the rare earth oxide be cerium oxide, lanthana,
At least one of yittrium oxide or ytterbium oxide.
4. the aluminium oxide ceramics according to any one of claim 1-3, it is characterised in that the particle diameter of the aluminum oxide is
20-50nm, purity are 99.99%；
The binding agent is at least one of paraffin, stearic acid, polyethylene and polypropylene.
5. a kind of preparation method of the aluminium oxide ceramics any one of claim 1-4, comprises the following steps：
1) by aluminum oxide, aluminium hydroxide, magnesia, kaolin, magnesium aluminate spinel and silane coupler mixed grinding in proportion, obtain
To compound；
2) after adhesive heating, then the compound is added thereto and mixed；
3) to step 2) processing after compound be molded, obtain article shaped；
4) carry out degumming successively to the article shaped, burn till, obtain aluminium oxide ceramics.
6. preparation method according to claim 5, it is characterised in that step 2) in, the temperature of the heating is 100-180
℃。
7. the preparation method according to claim 5 or 6, it is characterised in that step 3) in, it is described to be shaped to injection moulding.
8. preparation method according to claim 7, it is characterised in that the injection molding temperature is 150-190 DEG C, into
Type pressure is 2-4Mpa, and molding time is 5-10s.
9. the preparation method according to any one of claim 5-8, it is characterised in that step 4) in, the temperature of the degumming
Spend for 600-700 DEG C；
The temperature burnt till is 1200-1500 DEG C.
10. preparation method according to claim 9, it is characterised in that the temperature control burnt till is as follows：
(1) with 4-5h from room temperature to 600-700 DEG C；
(2) it is incubated 1-2h at 600-700 DEG C；
(3) it is warming up to 1200-1500 DEG C from 600-700 DEG C with 7-8h；
(4) it is incubated 15-20h at 1200-1500 DEG C.
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