CN112851310A - Preparation method of composite black ceramic - Google Patents
Preparation method of composite black ceramic Download PDFInfo
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- CN112851310A CN112851310A CN202110104810.1A CN202110104810A CN112851310A CN 112851310 A CN112851310 A CN 112851310A CN 202110104810 A CN202110104810 A CN 202110104810A CN 112851310 A CN112851310 A CN 112851310A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000012298 atmosphere Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 6
- 239000000049 pigment Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910000423 chromium oxide Inorganic materials 0.000 description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 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
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- 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
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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- 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
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- 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
- C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
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- 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
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Abstract
The invention discloses a preparation method of composite black ceramic, which is implemented according to the following steps: step 1, weighing the following raw materials in percentage by mass: al (Al)2O3：70％‑90％，Fe2O3：6％‑20％，TiO2: 3.8% -9%, Cu 0: 0.2-1 percent, and the sum of the contents of the raw materials is 100 percent; step 2, mixing the raw material powder weighed in the step 1 in proportion to obtain a mixed material; and 3, calcining and cooling the mixed material obtained in the step 2 under the condition of a specific sintering atmosphere to obtain the composite black ceramic. Solves the problem that Co is required to be used for making the ceramics black so far3O4、Cr2O3And the production cost is effectively reduced due to the problem of expensive materials.
Description
Technical Field
The invention belongs to the technical field of ceramics and ceramic pigments, and relates to a preparation method of composite black ceramics.
Background
With the increasing living standard of people, the requirements on the quality and the grade of porcelain products are also increased. For the ceramic product, the color of the ceramic can improve the service performance and play a role in decoration, and the like. Black is a color with various cultural meanings, and black ceramic products are always favored by people due to the characteristics of purity, elegance and high price in the decoration effect, and the development of black ceramic glaze with pure color and good chemical stability is always a popular topic for the research of ceramic pigment industry. Generally, the black ceramic can be prepared by adding oxides such as cobalt oxide and chromium oxide, but the oxides are expensive and limit the popularization of the black ceramic product. The present invention achieves a reduction in the production cost of black ceramics by designing a black ceramic composed of relatively inexpensive components.
Disclosure of Invention
The invention aims to provide a preparation method of composite black ceramic, which has the characteristics of excellent black performance and no need of adding high-price oxide.
The technical scheme adopted by the invention is that the preparation method of the composite black ceramic is implemented according to the following steps:
step 1, weighing the following raw materials in percentage by mass: al (Al)2O3：70％-90％，Fe2O3：6％-20％，TiO2: 3.8% -9%, CuO: 0.2-1 percent, and the sum of the contents of the raw materials is 100 percent;
step 2, mixing the raw material powder weighed in the step 1 by using a V-shaped mixer to obtain a mixed material;
and 3, calcining and cooling the mixed material obtained in the step 2 under the condition of a specific sintering atmosphere to obtain the composite black ceramic.
The invention is also characterized in that:
the particle size of each raw material in the step 1 is 5-45 μm.
The circularity of each raw material in the step 1 is 0.5-0.9.
The mixing time in step 2 is 30-45 minutes.
The sintering atmosphere in step 3 is specifically an air atmosphere or an inert gas atmosphere.
The calcination in step 3 specifically comprises heating and heat preservation.
The heating time for the temperature rise in the step 3 is 45-60min, and the temperature rise is up to 1040-1300 ℃.
The heat preservation time in the step 3 is 20-50 min.
The invention has the beneficial effects that:
1. the black ceramic prepared by the invention overcomes the defect that expensive oxide must be added in the traditional black ceramic production, greatly reduces the production cost, and efficiently prepares the black ceramic with pure color and good coloring performance.
2. The raw materials of the chemical reagents used in the invention are all powder, and no further mechanical crushing is needed after the powder pigment products are roasted, so that the preparation process steps are greatly simplified, and the production time is shortened. For products, the pressing and shaping are convenient, and the operation is simple. Therefore, the preparation method has great popularization value.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of composite black ceramic, which is implemented according to the following steps:
step 1, weighing the following raw materials in percentage by mass: al (Al)2O3：70％-90％，Fe2O3：6％-20％，TiO2: 3.8% -9%, CuO: 0.2-1 percent, and the sum of the contents of the raw materials is 100 percent; wherein the particle size of each raw material is 5-45 μm, and the circularity of each raw material is 0.5-0.9;
step 2, mixing the raw material powder weighed in the step 1 by using a V-shaped mixer for 30-45 minutes to obtain a mixed material;
and 3, calcining and cooling the mixed material obtained in the step 2 under the condition of air or inert gas sintering atmosphere to obtain the composite black ceramic, wherein the calcining specifically comprises heating and heat preservation, the heating time of the heating is 45-60min, the heating is carried out to 1040-1300 ℃, the heat preservation time is 20-50min, and the phase of the black ceramic is Al2O3、FeAlTiO5、Fe2O3、Cu2Al2O4And (4) forming.
Step 1, selecting small-particle-size high-circularity Al2O3，Fe2O3，TiO2CuO powder is beneficial to the full mixing of the powder, and the selected components abandon the traditional oxygenThe cobalt oxide, the chromium oxide and the like are expensive oxides, and low-price components are adopted, so that the production cost is greatly reduced;
step 2, mixing materials by using a V-shaped mixer to fully mix the materials;
step 3 under the heating temperature-rising and heat-preserving process selected by the invention, the phase of the sintered product is made of Al2O3、FeAlTiO5、Fe2O3、Cu2Al2O4The composition of the phase composition has high blackness and natural color.
Example 1
1.Al2O3-Fe2O3-TiO2-Cu0, the mass ratio of the components is 80% -12% -7.5% -0.5%;
2. weighing the powder according to the proportion in the step 1, mixing for 40 minutes by using a v-shaped mixer, and preparing to obtain a uniformly mixed material, wherein the average particle size of the powder is 15 mu m, and the average circularity is 0.65;
3. placing the mixed material in a heating furnace, and heating for 50min under the air atmosphere condition; when the temperature of the mixed materials is raised to 1200 ℃, preserving the heat for 30 min; then taking the material out of the heating furnace; air cooling to room temperature to obtain black ceramic. The CIE parameter of the prepared black ceramic is detected, and the result is as follows: the L value was 30.75, the a value was 0.01, and the b value was 0.62. The black ceramic prepared by the embodiment has high blackness and excellent effect.
Example 2
The difference from example 1 is that: selecting 74-16-9.1-0.9% of the components by mass ratio, and the other steps are the same as those in the embodiment 1.
The obtained black ceramic pigment has CIE parameters, and the result shows that the L value is 32.41, the a value is 0.12 and the b value is 0.10, which shows that the black ceramic prepared by the embodiment has high blackness and excellent effect.
Example 3
1.Al2O3-Fe2O3-TiO2-Cu0, selecting components with the mass ratio of 70% -20% -9% -1%;
2. weighing the powder according to the proportion in the step 1, mixing for 35 minutes by using a v-shaped mixer, and preparing to obtain a uniformly mixed material, wherein the average particle size of the powder is 28 microns, and the average circularity is 0.8;
3. placing the mixed material in a heating furnace, and heating for 55min under the condition of argon atmosphere; when the temperature of the mixed materials is raised to 1250 ℃, preserving the heat for 45 min; then taking the material out of the heating furnace; air cooling to room temperature to obtain black ceramic. The CIE parameter of the prepared black ceramic is detected, and the result is as follows: the L value was 30.81, the a value was 0.13 and the b value was-0.02. The black ceramic prepared by the embodiment has high blackness and excellent effect.
Example 4
1.Al2O3-Fe2O3-TiO2-Cu0, selecting 85-10-4.5-0.5% of the components by mass;
2. weighing the powder according to the proportion in the step 1, mixing for 30 minutes by using a v-shaped mixer, and preparing to obtain a uniformly mixed material, wherein the average particle size of the powder is 40 mu m, and the average circularity is 0.55;
3. placing the mixed material in a heating furnace, and heating for 45min under the condition of argon atmosphere; when the temperature of the mixed materials is increased to 1300 ℃, preserving the heat for 40 min; then taking the material out of the heating furnace; air cooling to room temperature to obtain black ceramic. The CIE parameter of the prepared black ceramic is detected, and the result is as follows: the L value was 30.51, the a value was-0.04, and the b value was 0.34. The black ceramic prepared by the embodiment has high blackness and excellent effect.
Example 5
1.Al2O3-Fe2O3-TiO2-Cu0, and the mass ratio of the selected components is 85-10-4.5-0.5%
2. Weighing the powder according to the proportion in the step 1, mixing for 30 minutes by using a v-shaped mixer, and preparing to obtain a uniformly mixed material, wherein the average particle size of the powder is 5 mu m, and the average circularity is 0.85;
3. placing the mixed material in a heating furnace, and heating for 60min under the air atmosphere condition; when the temperature of the mixed materials is increased to 1150 ℃, preserving the heat for 35 min; then taking the material out of the heating furnace; air cooling to room temperature to obtain black ceramic. The CIE parameter of the prepared black ceramic is detected, and the result is as follows: the L value was 34.01, the a value was-0.15, and the b value was-0.23. The black ceramic prepared by the embodiment has high blackness and excellent effect.
Claims (8)
1. The preparation method of the composite black ceramic is characterized by comprising the following steps:
step 1, weighing the following raw materials in percentage by mass: al (Al)2O3：70％-90％，Fe2O3：6％-20％，TiO2: 3.8% -9%, Cu 0: 0.2-1 percent, and the sum of the contents of the raw materials is 100 percent;
step 2, mixing the raw material powder weighed in the step 1 by using a V-shaped mixer to obtain a mixed material;
and 3, calcining and cooling the mixed material obtained in the step 2 under the condition of a specific sintering atmosphere to obtain the composite black ceramic.
2. The method for preparing a composite black ceramic according to claim 1, wherein the particle size of each raw material in step 1 is 5 μm to 45 μm.
3. The method for preparing a composite black ceramic according to claim 1, wherein the circularity of each raw material in step 1 is 0.5-0.9.
4. The method for preparing a composite black ceramic according to claim 1, wherein the mixing time in the step 2 is 30 to 45 minutes.
5. The method for preparing a composite black ceramic according to claim 1, wherein the sintering atmosphere in step 3 is specifically an air atmosphere or an inert gas atmosphere.
6. The method for preparing the composite black ceramic according to claim 1, wherein the calcining in the step 3 specifically comprises heating and holding.
7. The method as claimed in claim 5, wherein the heating time for the temperature rise in step 3 is 45-60min, and the temperature rise is 1040-1300 ℃.
8. The method for preparing the composite black ceramic according to claim 6, wherein the heat preservation time in the step 3 is 20-50 min.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050288166A1 (en) * | 2004-06-24 | 2005-12-29 | Jun-Kyu Cha | Lead-free black ceramic composition for filter and filter formed using the same |
| CN103189331A (en) * | 2010-11-01 | 2013-07-03 | 昭和电工株式会社 | Method for producing alumina sintered body, alumina sintered body, abrasive grains, and grindstone |
| US20150307406A1 (en) * | 2012-12-21 | 2015-10-29 | Rolex S.A. | Coloured technical ceramic bodies and method for preparing the same |
| CN110330315A (en) * | 2019-07-04 | 2019-10-15 | 新化县顺达电子陶瓷有限公司 | A kind of low-temperature sintered alumina black ceramic and preparation method thereof |
| CN110723977A (en) * | 2019-08-23 | 2020-01-24 | 东北大学秦皇岛分校 | With Cu2+Formation of black CuAl in alumina porcelain2O4Method for preparing black alumina ceramic by using main colorant |
| JP2020180020A (en) * | 2019-04-25 | 2020-11-05 | 京セラ株式会社 | Black ceramics |
-
2021
- 2021-01-26 CN CN202110104810.1A patent/CN112851310A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050288166A1 (en) * | 2004-06-24 | 2005-12-29 | Jun-Kyu Cha | Lead-free black ceramic composition for filter and filter formed using the same |
| CN103189331A (en) * | 2010-11-01 | 2013-07-03 | 昭和电工株式会社 | Method for producing alumina sintered body, alumina sintered body, abrasive grains, and grindstone |
| US20150307406A1 (en) * | 2012-12-21 | 2015-10-29 | Rolex S.A. | Coloured technical ceramic bodies and method for preparing the same |
| JP2020180020A (en) * | 2019-04-25 | 2020-11-05 | 京セラ株式会社 | Black ceramics |
| CN110330315A (en) * | 2019-07-04 | 2019-10-15 | 新化县顺达电子陶瓷有限公司 | A kind of low-temperature sintered alumina black ceramic and preparation method thereof |
| CN110723977A (en) * | 2019-08-23 | 2020-01-24 | 东北大学秦皇岛分校 | With Cu2+Formation of black CuAl in alumina porcelain2O4Method for preparing black alumina ceramic by using main colorant |
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Application publication date: 20210528 |