CN116621564A - Pure black large-size alumina ceramic structural member and preparation method thereof - Google Patents
Pure black large-size alumina ceramic structural member and preparation method thereof Download PDFInfo
- Publication number
- CN116621564A CN116621564A CN202310367368.0A CN202310367368A CN116621564A CN 116621564 A CN116621564 A CN 116621564A CN 202310367368 A CN202310367368 A CN 202310367368A CN 116621564 A CN116621564 A CN 116621564A
- Authority
- CN
- China
- Prior art keywords
- pure black
- alumina ceramic
- structural member
- black
- ceramic structural
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000003086 colorant Substances 0.000 claims abstract description 6
- 239000000292 calcium oxide Substances 0.000 claims abstract description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 238000003825 pressing Methods 0.000 claims abstract description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 16
- 239000011812 mixed powder Substances 0.000 claims description 9
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 5
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 4
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 12
- 238000010304 firing Methods 0.000 abstract description 8
- 230000001681 protective effect Effects 0.000 abstract description 4
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 238000007873 sieving Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 239000012856 weighed raw material Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- -1 cutting tool Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007676 flexural strength test Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3275—Cobalt oxides, cobaltates or cobaltites or oxide forming salts thereof, e.g. bismuth cobaltate, zinc cobaltite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/95—Products characterised by their size, e.g. microceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9661—Colour
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The application discloses a preparation method of a pure black large-size alumina ceramic structural member, and belongs to the technical field of ceramic materials. The pure black large-size alumina ceramic structural member comprises the following raw materials in percentage by mass: 90-95% Al 2 O 3 1.5 to 7.5 percent of colorant and 1 to 2.5 percent of calcium oxide and/or magnesium oxide, ball milling the weighed raw materials of each component, sieving, dry pressing and molding, and firing by using a common electric furnace at a constant speed and heating to 1580 ℃ to obtain the pure black alumina ceramic material. The pure black large-size alumina ceramic structural member prepared by the application has the thickness of not less than 20mm, the length and width or diameter size of 20cm-90cm, uniform color, pure black consistent inside and outside, high heat conductivity and high flexural strength. The preparation method provided by the application can be used for firing pure black alumina ceramics with consistent inside and outside without using a special kiln or in a protective gas and oxidizing flame, and has good practicability.
Description
Technical Field
The application belongs to the technical field of ceramic materials, and particularly relates to a pure black large-size aluminum oxide ceramic structural member and a preparation method thereof.
Background
The alumina ceramic has the characteristics of high strength, high hardness, wear resistance, corrosion resistance, high temperature resistance, good thermal conductivity, high insulation, low dielectric loss, stable electrical property and the like. It can be made into integrated circuit substrate, cutting tool, acid and alkali resistant piece, artificial skeleton, grinding material, high-grade refractory material and fluorescent powder carrier, etc. and can be extensively used in the industries of electronics, machinery, chemical industry, medicine, photoelectricity, aerospace and aviation, etc. The pure black alumina ceramic has a series of excellent performances of light shielding property, good air tightness, high mechanical strength, high hardness, abrasion resistance, high temperature resistance, good insulativity, acid and alkali resistance and the like, and is more and more widely applied to military products and civil products, and some irreplaceable characteristics of the pure black alumina ceramic lead the pure black alumina ceramic to have wide market prospect and development space. Based on these advantages of pure black alumina ceramics, pure black alumina ceramics are currently widely used for manufacturing package cases for semiconductor integrated circuits.
At present, the black alumina ceramics are generally prepared by a primary synthesis method and a secondary synthesis method at home and abroad. Wherein, the primary synthesis method is to directly prepare black alumina ceramics by alumina, coloring oxide and auxiliary agent according to a certain proportion and process. CN 105669169A discloses a black alumina ceramic, a method for manufacturing the same, and an alumina ceramic device, wherein the method for manufacturing the black alumina ceramic has the advantages of low sintering temperature, stable size and high yield, and the prepared black alumina ceramic has uniform pure black color. However, the black toner used in this patent does not include chromium, and according to the present inventors' various experimental attempts, the black toner does not use chromium-burned pure black alumina ceramics, which causes a phenomenon of black appearance and red-brown inside; pre-firing is required before firing, and the process is troublesome to fire; the black alumina ceramic is prepared by sintering in a protective atmosphere, so that the productivity is low, the firing color of a large product is uneven, the inside and outside are inconsistent, the yield is low, the production requirement cannot be met, the firing cost of a small amount of products is too high, and the flexibility is poor.
Disclosure of Invention
Aiming at the problems in the prior art, the application aims to provide a preparation method of a pure black large-size alumina ceramic structural member, and the pure black large-size alumina ceramic structural member prepared by the method has consistent pure black inside and outside and high yield.
In order to solve the technical problems, the technical scheme adopted by the application is as follows:
a preparation method of a pure black large-size alumina ceramic structural member comprises the following steps:
1) Weighing the following raw materials in percentage by mass: 90-95% Al 2 O 3 1.5 to 7.5 percent of colorant and 1 to 2.5 percent of calcium oxide and/or magnesium oxide, and drying for standby;
2) Ball milling is carried out in batches after the balls are mixed with the raw materials in proportion to obtain black mixed powder;
3) And (3) dry-pressing the black mixed powder to form, putting the black mixed powder into a common electric furnace, controlling the temperature to 1580 ℃ for oxidizing flame sintering, preserving the heat for more than 1h, and naturally cooling to obtain the pure black alumina ceramic.
The colorant is one or more selected from ferric oxide, manganese oxide and cobalt oxide.
In the step 2), ball milling is carried out on the balls and the raw materials in batches according to the proportion of 1:1.2, the ball milling speed is 40-50 r/min, and the ball milling time is 16-25 hours.
In the step 3), after ball milling, sieving with a 300-mesh sieve to obtain black mixed powder.
In the step 4), the plate formed by pressing is placed into a common electric ceramic furnace, the temperature is raised to 500 ℃ at the speed of 1 ℃/3min, the temperature is raised to 1000 ℃ at the speed of 2 ℃/5min, the temperature is raised to 1580 ℃ at the speed of 1 ℃/min, the temperature is kept for more than 1h, and the pure black alumina ceramic is obtained after natural cooling.
The pure black large-size alumina ceramic structural member prepared by the method.
Compared with the prior art, the application has the technical advantages that:
1) The thickness of the pure black large-size alumina ceramic structural member prepared by the application is not less than 20mm, can reach more than 30mm, the length and width or diameter size can reach 20cm-90cm, the color is uniform, the inside and outside are uniform, the pure black ceramic structural member has high heat conductivity, high breaking strength and good packaging combination, and can meet the production requirements in special environments.
2) According to the preparation method of the pure black large-size alumina ceramic structural member, when black alumina ceramics with various sizes are fired, special kilns are not needed, and pure black alumina ceramics with consistent inside and outside can be fired without using protective gas and oxidizing flame.
Drawings
The left diagram of FIG. 1 is a diagram of a pure black large-size alumina ceramic structural member prepared by the application, and the right diagram is a diagram of a reddish alumina ceramic prepared by Japanese company.
Detailed Description
The application is further described below in connection with specific embodiments. These examples are only for illustrating the present application and are not intended to limit the scope of the present application. Modifications and substitutions to methods, procedures, or conditions of the present application without departing from the spirit and nature of the application are intended to be within the scope of the present application. In the following examples, unless otherwise indicated, all technical means used in the examples are conventional means well known to those skilled in the art.
Example 1
A pure black large-size alumina ceramic structural member was prepared according to the raw material amount of Table 1, wherein the large specification was a square or round ceramic structural member having a length, width or diameter of 200mm or more and a thickness of 20mm or more. The product prepared in this example has dimensions of 750mm long by 250mm wide and a thickness of 25mm.
The preparation method comprises the following specific steps:
1) Al is added with 2 O 3 Mixing colorant (selected from ferric oxide, manganese oxide, and cobalt oxide), calcium oxide and/or magnesium oxide, and oven drying;
2) Ball milling is carried out on the balls and the raw materials in batches according to the proportion of 1:1.2, the ball milling speed is 40-50 r/min, and the ball milling time is 16-25 hours;
3) Sieving with 300 mesh sieve after ball milling to obtain black mixed powder, and dry-pressing under 600 ton pressure;
4) And (3) placing the pressed plate into a common electric ceramic furnace, heating to 1580 ℃ at the speed of 3 ℃/2.5min, preserving heat for 1h, and naturally cooling to obtain the pure black alumina ceramic.
TABLE 1 product composition and amounts (parts by weight) and test results
| Product 1 | Product 2 | Product 3 | Product 4 | Comparative 1 | Comparative example 2 | |
| Al 2 O 3 | 90％ | 92％ | 92％ | 95％ | 92％ | 92％ |
| CaO | 1.5％ | 1％ | 1％ | 0.5％ | 0 | 0 |
| MgO | 1％ | 1％ | 1％ | 0.5％ | 0 | 0 |
| Na 2 O | 0 | 0 | 0 | 0 | 1.5％ | 1％ |
| K 2 O | 0 | 0 | 0 | 0 | 1％ | 1.5％ |
| Iron oxide | 3.5％ | 4％ | 4％ | 2％ | 1.5％ | 0 |
| Manganese oxide | 1.5％ | 1％ | 0.5％ | 1％ | 0 | 0 |
| Cobalt oxide | 2.5％ | 1％ | 1.5％ | 1％ | 0 | 0 |
| Nickel oxide | 0 | 0 | 0 | 0 | 2％ | 3.5 |
| Titanium oxide | 0 | 0 | 0 | 0 | 2％ | 2 |
| Purity of black | Pure black | Pure black | Pure black | Pure black | Internal black and red | Internal black and red |
| Yield of percent of pass | 97％ | 96％ | 99％ | 94％ | 85％ | 82％ |
| Flexural Strength | 75MPa | 82MPa | 85MPa | 76MPa | 57MPa | 63MPa |
| Shrinkage rate | 1.1％ | 1.08％ | 0.9％ | 1.0％ | 1.5％ | 1.8％ |
Wherein, the flexural strength is carried out by adopting a GB/T3001-2007 refractory material normal temperature flexural strength test method, and the thickness of the test product is 1mm (the test is carried out by adopting the small sample prepared by the method of the embodiment). The black purity is obtained by directly observing and comparing the cross section of the product with naked eyes, and the qualified product is the product without cracks after sintering.
As shown in FIG. 1, the pure black alumina ceramic (product 1) prepared by the application has uniform color and pure black color; the inner and outer surfaces are consistent with pure black, the problem of black appearance and red coffee color inside is solved, and the mirror surface can be polished.
As can be seen from table 1, the specifications of the raw materials, the specific components of the product and the reasonable amounts thereof are one of the main factors determining the black color of the product, and the effect of the black purity of the product 3 in this example is most prominent compared with other products.
Example 2
Product 3 was prepared as in example 1, except that the shrinkage, cracking ratio and whether the finished product was porcelain or not were each examined according to the temperature programming in table 2.
TABLE 2 different preparation methods and detection results of the products
As shown in Table 2, the product of the application is sintered by using a common electric furnace and is fired by oxidizing flame at a stepwise constant temperature rise, the pre-firing is not required, and the protective atmosphere is not required to be introduced in the firing process, so that the qualification rate of the product can be greatly improved.
Claims (6)
1. The preparation method of the pure black large-size alumina ceramic structural member is characterized by comprising the following steps of:
1) Weighing the following raw materials in percentage by mass: 90-95% Al 2 O 3 1.5 to 7.5 percent of colorant and 1 to 2.5 percent of calcium oxide and/or magnesium oxide, and drying for standby;
2) Ball milling is carried out in batches after the balls are mixed with the raw materials in proportion to obtain black mixed powder;
3) And (3) dry-pressing the black mixed powder to form, putting the black mixed powder into a common electric furnace, controlling the temperature to 1580 ℃ for oxidizing flame sintering, preserving the heat for more than 1h, and naturally cooling to obtain the pure black alumina ceramic.
2. The method for preparing a pure black large-size alumina ceramic structural member according to claim 1, wherein the colorant is one or more selected from the group consisting of iron oxide, manganese oxide and cobalt oxide.
3. The method for preparing a pure black large-sized alumina ceramic structural member according to claim 1, wherein in the step 2), balls and raw materials are subjected to ball milling in batches according to a ratio of 1:1.2, wherein the ball milling speed is 40-50 rpm, and the ball milling time is 16-25 hours.
4. The method for preparing a pure black large-size alumina ceramic structural member according to claim 1, wherein in the step 3), after ball milling, the powder is sieved by a 300-mesh sieve to obtain black mixed powder.
5. The method for preparing the pure black large-size alumina ceramic structural member according to claim 1, wherein in the step 4), the pressed plate is put into a common electroceramic furnace to be heated to 500 ℃ at a speed of 1 ℃/3min, heated to 1000 ℃ at a speed of 2 ℃/5min, heated to 1580 ℃ at a speed of 1 ℃/min, and kept for more than 1 hour, and naturally cooled to obtain the pure black alumina ceramic.
6. The pure black large-size alumina ceramic structural member prepared by the method of any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310367368.0A CN116621564A (en) | 2023-04-07 | 2023-04-07 | Pure black large-size alumina ceramic structural member and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310367368.0A CN116621564A (en) | 2023-04-07 | 2023-04-07 | Pure black large-size alumina ceramic structural member and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116621564A true CN116621564A (en) | 2023-08-22 |
Family
ID=87640663
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310367368.0A Pending CN116621564A (en) | 2023-04-07 | 2023-04-07 | Pure black large-size alumina ceramic structural member and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116621564A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05238810A (en) * | 1992-02-27 | 1993-09-17 | Onoda Cement Co Ltd | Black alumina sintered compact |
| CN105669169A (en) * | 2016-01-28 | 2016-06-15 | 深圳市商德先进陶瓷有限公司 | Black alumina ceramic, manufacturing method thereof and alumina ceramic device |
| CN107406328A (en) * | 2015-03-19 | 2017-11-28 | 衡所华威电子有限公司 | Alumina ceramic of black color powder, alumina ceramic of black color body prepared therefrom and the method for preparing the alumina ceramic of black color body |
| CN109111760A (en) * | 2018-07-12 | 2019-01-01 | 江西赛瓷材料有限公司 | A kind of alumina ceramic of black color toner and its preparation method and application |
-
2023
- 2023-04-07 CN CN202310367368.0A patent/CN116621564A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05238810A (en) * | 1992-02-27 | 1993-09-17 | Onoda Cement Co Ltd | Black alumina sintered compact |
| CN107406328A (en) * | 2015-03-19 | 2017-11-28 | 衡所华威电子有限公司 | Alumina ceramic of black color powder, alumina ceramic of black color body prepared therefrom and the method for preparing the alumina ceramic of black color body |
| CN105669169A (en) * | 2016-01-28 | 2016-06-15 | 深圳市商德先进陶瓷有限公司 | Black alumina ceramic, manufacturing method thereof and alumina ceramic device |
| CN109111760A (en) * | 2018-07-12 | 2019-01-01 | 江西赛瓷材料有限公司 | A kind of alumina ceramic of black color toner and its preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| 焦宝祥: "《无机非金属材料工艺学》", 31 May 2011, 华东理工大学出版社, pages: 228 - 229 * |
| 王迎军等: "新型材料科学与技术 无机材料卷 上", 31 October 2016, 华南理工大学出版社, pages: 89 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110330315B (en) | Low-temperature sintered alumina black ceramic and preparation method thereof | |
| CN102795894A (en) | Surface metallization layer of high-purity alumina ceramics and compounding technology thereof | |
| CN103755361A (en) | Aluminum-chromium-silicon fireproof material | |
| CN111233482A (en) | High-temperature-resistant sagger and preparation method thereof | |
| CN115259902A (en) | High-temperature stable green rare earth infrared radiation coating and preparation method and application thereof | |
| CN110028316B (en) | Cordierite kiln furniture sagger and preparation method thereof | |
| CN105669169A (en) | Black alumina ceramic, manufacturing method thereof and alumina ceramic device | |
| CN111470871A (en) | Preparation method of low-temperature co-fired ceramic superhard abrasive polymer based on 3D printing | |
| CN107619286A (en) | A kind of preparation method of corundum-mullite sagger | |
| CN104310976A (en) | Highly wear-resistant high-temperature ceramic | |
| CN109020521B (en) | Compact chromium oxide brick and manufacturing method thereof | |
| CN114031297A (en) | Cordierite-based porous glass ceramic and preparation method thereof | |
| CN102992783B (en) | Corundum brick used for gas channel parts of bottle, can, glass kiln and combustion chamber of rangette | |
| CN116621564A (en) | Pure black large-size alumina ceramic structural member and preparation method thereof | |
| CN112430104A (en) | Composite additive for preparing ceramic and preparation method and application thereof | |
| CN104876608A (en) | Manufacturing method of thermal-shock resistant refractory brick | |
| CN102951913A (en) | Isostatic compaction corundum spinel crucible and preparation method thereof | |
| CN113526946B (en) | High-toughness modified silicon corundum brick | |
| CN112521135A (en) | Low-temperature sintered Al2O3Microwave dielectric material | |
| CN110550941B (en) | High-temperature-resistant non-oxidized graphite ceramic material | |
| KR102650353B1 (en) | Refractory batch, method for producing irregular refractory ceramic product from said batch and irregular refractory ceramic product obtained by said method | |
| KR100421435B1 (en) | Method of manufact uring and ceramic sheet for heat to high strength and high heat conduction | |
| CN107805071B (en) | Preparation method of titanium-trialuminum-carbon-mullite composite ceramic with low glass wettability | |
| CN111995415A (en) | Composite boron nitride ceramic high-temperature nozzle and preparation method thereof | |
| CN110862261A (en) | Yellow zirconia ceramic powder and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |