CN1772703A - Prepn process of heterogenous TiN/(Ca, Mg) alpha'-sialon ceramic material with titanium-containing blast furnace slag - Google Patents
Prepn process of heterogenous TiN/(Ca, Mg) alpha'-sialon ceramic material with titanium-containing blast furnace slag Download PDFInfo
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Abstract
The preparation process of heterogenous TiN/(Ca, Mg) alpha'-Sialon ceramic material with titanium-containing blast furnace slag includes two steps. The first step of synthesizing TiN/(Ca, Mg) alpha'-Sialon powder includes crushing, ball grinding, sieving, magnetic separating, compounding material with titanium-containing blast furnace slag, silica fume, bauxite and carbon black in certain weight proportion, wet mixing, drying, dry mixing, molding to form, high temperature sintering and burning out residual carbon. The second step of preparing heterogenous TiN/(Ca, Mg) alpha'-Sialon ceramic material includes mixing the synthesized TiN/(Ca, Mg) alpha'-Sialon powder with additive calcium carbonate, single axial molding to form, and high temperature sintering at 1600-1700 deg.c inside high temperature furnace. The product has excellent performance and the preparation process is simple, low in production cost and environment friendly.
Description
Technical field
The present invention relates to a kind of preparation method of composite diphase material, be specifically related to utilize titanium-containing blast furnace slag to prepare TiN/ (Ca, Mg) method of α '-Sialon diphase ceramic material.
Background technology
Do not see as yet both at home and abroad at present and utilize titanium-containing blast furnace slag to prepare TiN/ (Ca, Mg) any report of α '-Sialon diphase ceramic material.Single-phase α '-Sialon and α '-Sialon base composite diphase material is many to be that raw material passes through reaction sintering (RS) preparation with pure nitride and oxide compound.Though this method can be prepared the higher material of purity, the raw materials cost height, complex process is not suitable for industrial-scale production.In addition, also having with natural mineral or industrial residue is that raw material prepares α '-Sialon from spreading sintering process (SHS), though this method reaction times is short, speed is fast, is not suitable for industrial-scale production equally, and the poor reproducibility of sintered products.Titanium-containing blast furnace slag is big owing to its quantity discharged as a kind of waste residue of metallurgy industry, and utilization ratio is low, environment has been caused bigger pollution.Therefore, no matter from still ecological first-class aspect consideration economically, all need blast furnace slag is carried out the utilization of mass efficient.
Summary of the invention
At the defective of prior art, the purpose of this invention is to provide a kind of low-cost preparation of titanium-containing blast furnace slag TiN/ (Ca, Mg) method of α '-Sialon diphase ceramic material utilized.Promptly utilize output titanium-containing blast furnace slag huge, with low cost to be main raw material, adjust composition, adopt the carbothermal reduction-nitridation legal system to be equipped with TiN/ (Ca, Mg) α '-Sialon diphase ceramic material with silicon ash and bauxitic clay.It is simple and easy to do not only to reach technology, and suitable industrialization continuous production, reduce TiN/ (Ca greatly, Mg) preparation cost of α '-Sialon diphase ceramic material, do not provide a new way for China's titanium-containing blast furnace slag has new integral body utilization discarded and pollution and ecology, reduce pollution environment.
Realize the technical scheme of the object of the invention: with TiO
2Content is that 22～26% titanium-containing blast furnace slag is a main raw material, uses SiO
2Content is 82～90% silicon ash and Al
2O
3Content is that 79～85% bauxitic clay is adjusted composition, and carbon black is a reductive agent, produce in two steps TiN/ (Ca, Mg) α '-Sialon diphase ceramic material:
The first step: synthetic TiN/ (Ca, Mg) α '-Sialon powder
(1) fragmentation: block titanium-containing blast furnace slag is carried out fragmentation, handle obtaining ground-slag then with the slag of sampling machine after to fragmentation;
(2) ball milling: the ground-slag bigger to above-mentioned granularity carries out fine grinding;
(3) sieve: sieve with the ground-slag of 200 purpose standard sieves after to above-mentioned fine grinding;
(4) magnetic separation: with magnet ground-slag is carried out magnetic separation, remove contained fe and ferromagnetic material in the ground-slag;
(5) batching: the chemical formula of selected synthetic α '-Sialon be (Ca, Mg)
xSi
12-3xAl
3xO
xN
16-x, x=0.3 in the formula～2.0 determine that the quality per distribution ratio of raw material is: titanium-containing blast furnace slag 5.22～31.98%, silicon ash 18.88～65.71%, bauxitic clay 3.66～24.41%, carbon black 23.06～43.19%;
(6) wet mixing: with prepared mixture is that medium is mixed into slip with the dehydrated alcohol, and the wet mixing time is 24 hours;
(7) drying: the slip after the wet mixing is put into baking oven in 60 ℃ of oven dry down;
(8) dried mixing: dried compound is done and was mixed 4 hours, and places moisture eliminator to preserve the gained blank;
(9) compression molding: the blank that will do after mixing carries out single shaft to compression moulding, and forming pressure is 25MPa, pressurize 1min;
(10) high temperature burns till: the blank of compression moulding is put into plumbago crucible, use MoSi
2High temperature resistance furnace heating is that 1450～1500 ℃, constant temperature time are that 6～10 hours, intensification and cooling rate are to feed continuously all the time in the stove under the flowing nitrogen condition that flow is 400～800ml/min in 3～5 ℃/min, the sintering process and carry out sintering at a normal atmosphere, firing temperature;
(11) burning-off carbon residue: with the above-mentioned TiN/ that sinters into (Ca, Mg) α '-Sialon powder places in the retort furnace, constant temperature was heat-treated in 6 hours in 580 ℃ of air, removed remaining uncombined carbon;
Second step: TiN/ (Ca, Mg) preparation of α '-Sialon diphase ceramic material
With the first step synthetic TiN/ (Ca, Mg) α '-Sialon powder and the addition of C aCO that accounts for raw material gross weight 10～15%
3Thorough mixing is even, is 200MPa at pressure, and single shaft is to compression molding, and pressurize 1min puts into plumbago crucible with these green compact then and imbeds by 60%Si
3N
4In the powder mix that+30%AlN+10%BN forms; place sintering oven, under the high pure nitrogen protection, carry out normal pressure, high temperature sintering; sintering temperature is 1600～1700 ℃; be incubated 1～2 hour; intensification is to take temperature increasing schedule stage by stage; heat-up rate is 5～30 ℃/min, and cooling rate is 30～40 ℃/min.
High temperature sintering described in second step is taked stage by stage, and temperature increasing schedule is: the speed with 25～30 ℃/min heats up earlier, when temperature reaches 1150 ℃, the insulation 30min, be warming up to 1400 ℃ with 25～30 ℃/min speed subsequently after, the speed with 5～10 ℃/min rises to sintering temperature again; Described sintering oven is a vacuum carbon tube furnace.
Significant advantage of the present invention and positively effect are:
1, having made full use of output titanium-containing blast furnace slag big, with low cost is main raw material, and therefore, not only production cost is very low, and has opened up new approach for the utilization of a large amount of depleted titanium-containing blast furnace slags of China, has reduced the pollution to environment.
2, the present invention utilizes titanium-containing blast furnace slag to be main raw material, and (technology is simple for Ca, Mg) α '-Sialon diphase ceramic material, and the material middle long column shape α '-Sialon crystal grain that obtains has significantly from toughening effect this material for synthetic TiN/.Simultaneously because the TiO in the titanium-containing blast furnace slag
2The TiN particle that obtains behind the reduction nitridation is tiny, and the fusing point height, and hardness has high electrical conductivity greatly again, improved the over-all properties of synthetic materials.This product has various premium propertiess: (1) belongs to low density, high rigidity, high-strength material.Volume density is 2.41～2.52g/cm
3, Vickers' hardness is 12～17GPa, normal temperature ultimate compression strength is 423～537MPa; (2) resistivity at room temperature is about 10
6Ω cm belongs to semi-conductor.(3) has anti-preferably atmospheric oxidation performance.In air " passive oxidation " can take place, sample is outer to form " protective membrane ", stops further carrying out of oxidizing reaction.
Embodiment
Example 1: the first step is synthesized TiN/ (Ca, Mg) α '-Sialon powder.At first titanium-containing blast furnace slag is carried out fragmentation, handle obtaining ground-slag then with the slag of sampling machine after, again ground-slag is put into the fine grinding of urethane ball grinder, reach below 200 meshes until the ground-slag granularity to fragmentation.Ground-slag after the screening is carried out magnetic separation to remove contained fe and ferromagnetic material in the slag.Titanium-containing blast furnace slag after the magnetic separation is mixed with silicon ash, bauxitic clay, carbon black, and its proportioning is: titanium-containing blast furnace slag is 26.02g, and the silicon ash is 22.82g, and bauxitic clay is 19.83g, and carbon black is 31.33g.Prepared mixture is placed the urethane ball grinder, is medium wet mixing 24h with the dehydrated alcohol, then slip is put into baking oven in 60 ℃ of oven dry down.Do again after the material thorough drying to be mixed and mix 4h, full and uniform to guarantee compound.The blank of doing after mixing is put into punching block, be pressed into the roundlet base of Φ 15mm in 25MPa down with single shaft to machine.Biscuit after the mold pressing is packed in the plumbago crucible, place vertical MoSi
2In the resistance furnace zone of constant temperature, feed nitrogen (N%＞99%) continuously by furnace bottom, carry out sintering under the normal pressure, (Asia-Pacific, Shanghai precision meter factory) carries out temperature control with XMTA-1 type temperature controller, the about 5 ℃/min of heat-up rate, the about 4 ℃/min of cooling rate.Sintering temperature is 1480 ℃, and constant temperature 8h, nitrogen flow are 400ml/min.Sample after burning till is placed on grind into powder in the agate mortar, is placed in the inherent 580 ℃ of air of retort furnace constant temperature then and heat-treated in 6 hours, to remove remaining uncombined carbon.Detected result shows: main thing contains a small amount of SiC and β-CaSiO in addition mutually for α '-Sialon, AlN and TiN in the synthetic powder
3
Second step preparation TiN/ (Ca, Mg) α '-Sialon diphase ceramic material.Earlier with above-mentioned powder and the addition of C aCO that accounts for powder quality 10%
3Doing in agate mortar and mix 0.5h, is medium wet mixing 1h again with the dehydrated alcohol, then slip is put into baking oven in 60 ℃ of oven dry down.Do again after the material thorough drying to be mixed and mix 0.5h, full and uniform to guarantee compound.Again blank is put into punching block, under 200MPa, becoming diameter with single shaft to the machine dry-pressing is the roundlet base of 12mm.Biscuit after the mold pressing is packed in the plumbago crucible, place vacuum carbon tube furnace at the high pure nitrogen atmosphere with bury powder (60wt%Si
3N
4+ 30wt%AlN+10%wtBN) carry out under the condition normal pressure-sintered.1700 ℃ of sintering temperatures, insulation 2h, constant temperature precision ± 1 ℃.Heat-up rate is that 25 ℃/min heats up, and insulation 0.5h when temperature rises to 1150 ℃ is to guarantee addition of C aCO
3Fully decompose, be warming up to 1400 ℃ with 30 ℃/min speed then after, rise to sintering temperature with 5 ℃/min speed again, begin cooling behind the insulation 1.5h, cooling rate is 30 ℃/min.Detected result shows: and synthetic TiN/ (Ca, Mg) main thing be α '-Sialon and TiN mutually in α '-Sialon diphase ceramic material, minute quantity SiC and impurity is mutually in addition in addition.This diphase ceramic material volume density is 2.52g/cm
3, Vickers' hardness is 17GPa, and normal temperature ultimate compression strength is 537MPa, and resistivity at room temperature is about 2.54 * 10
6Ω cm belongs to semiconductor material.Behind 1300 ℃ of oxidation 3h, the unit surface oxidation weight gain is 12.41mg/cm
2
Example 2: the first step is synthesized TiN/ (Ca, Mg) α '-Sialon powder.Preparation of raw material is: getting titanium-containing blast furnace slag is 29.06g, and the silicon ash is 25.48g, and bauxitic clay is 22.15g, and carbon black is 23.31g.1500 ℃ of sintering temperatures, constant temperature 6h, heat-up rate are 3 ℃/min, nitrogen flow is 600ml/min.Second step preparation TiN/ (Ca, Mg) α '-Sialon diphase ceramic material: with above-mentioned powder and the addition of C aCO that accounts for powder quality 15%
3In agate mortar, do and mix 0.5h; 1650 ℃ of sintering temperatures, insulation 1h.Temperature increasing schedule is: when rising to 1150 ℃ with 30 ℃/min speed, insulation 0.5h, after rising to 1600 ℃ with 28 ℃/min speed then, rise to sintering temperature with 10 ℃/min speed again, behind the insulation 1h, begin the cooling, cooling rate is 40 ℃/min, more than two the step other technological processs and processing condition with embodiment 1.Detected result shows: main thing contains a small amount of 15R, SiC and β-CaSiO in addition mutually for α '-Sialon, AlN and TiN in the synthetic powder
3Synthetic TiN/ (Ca, Mg) main thing is α '-Sialon and TiN mutually in α '-Sialon diphase ceramic material, this diphase ceramic material volume density is 2.51g/cm
3, Vickers' hardness is 15GPa, and normal temperature ultimate compression strength is 512MPa, and resistivity at room temperature is about 5.68 * 10
6Ω cm belongs to semiconductor material.Behind 1300 ℃ of oxidation 3h, the unit surface oxidation weight gain is 13.79mg/cm
2
Example 3: the first step is synthesized TiN/ (Ca, Mg) α '-Sialon powder.Preparation of raw material is: getting titanium-containing blast furnace slag is 10.27g, and the silicon ash is 57.18g, and bauxitic clay is 7.58g, and carbon black is 24.97g.1450 ℃ of sintering temperatures, constant temperature 10h, nitrogen flow are 800ml/min.Second step preparation TiN/ (Ca, Mg) α '-Sialon diphase ceramic material.1600 ℃ of sintering temperatures, insulation 2h.Temperature increasing schedule is: when rising to 1150 ℃ with 27 ℃/min speed, the insulation 0.5h, rise to 1400 ℃ with 30 ℃/min speed then after, the speed with 7 ℃/min rises to sintering temperature again, the insulation 1.5h after, begin the cooling, cooling rate is 35 ℃/min.More than two the step other processing steps and processing condition with embodiment 1.Detected result shows: main thing contains a small amount of SiC and β-CaSiO in addition mutually for α '-Sialon and TiN in the synthetic powder
3Synthetic TiN/ (Ca, Mg) main thing is α '-Sialon and TiN mutually in α '-Sialon diphase ceramic material, this diphase ceramic material volume density is 2.41g/cm
3, Vickers' hardness is 12GPa, and normal temperature ultimate compression strength is 423MPa, and resistivity at room temperature is about 9.37 * 10
6Ω cm belongs to semiconductor material.Behind 1300 ℃ of oxidation 3h, the unit surface oxidation weight gain is 15.13mg/cm
2
Example 4: the first step is synthesized TiN/ (Ca, Mg) α '-Sialon powder.Preparation of raw material is: getting titanium-containing blast furnace slag is 5.22g, and the silicon ash is 65.71g, and bauxitic clay is 3.66g, and carbon black is 25.41g.Other processing step in the first step and second step is all identical with embodiment 1 with processing condition with processing step, final detection result: in the synthetic powder mainly thing be α '-Sialon and TiN mutually, contain a small amount of SiC and impurity in addition mutually.This diphase ceramic material volume density is 2.45g/cm
3, Vickers' hardness is 15GPa, and normal temperature ultimate compression strength is 430MPa, and resistivity at room temperature is about 5.70 * 10
6Ω cm belongs to semiconductor material.Behind 1300 ℃ of oxidation 3h, the unit surface oxidation weight gain is 12.52mg/cm
2
Example 5: (Ca, Mg) the first step of α '-Sialon diphase ceramic material is all identical with example 1 with processing condition with the processing step in second step to produce TiN/.Different is the synthetic TiN/ of the first step (Ca, Mg) in α '-Sialon powder process, preparation of raw material is: getting titanium-containing blast furnace slag is 16.78g, the silicon ash is 46.19g, bauxitic clay is 12.63g, carbon black is 24.40g.Final detection result: main thing is α '-Sialon and TiN mutually in the synthetic powder, contains a small amount of SiC and impurity in addition mutually.This diphase ceramic material volume density is 2.50g/cm
3, Vickers' hardness is 16GPa, and normal temperature ultimate compression strength is 533MPa, and resistivity at room temperature is about 2.65 * 10
6Ω cm belongs to semiconductor material.Behind 1300 ℃ of oxidation 3h, the unit surface oxidation weight gain is 12.91mg/cm
2
Example 6: (Ca, Mg) the first step of α '-Sialon diphase ceramic material is identical with example 1 with processing condition with the processing step in second step to produce TiN/.Different is that raw material is formulated as in the first step: getting titanium-containing blast furnace slag is 23.04g, and the silicon ash is 35.63g, and bauxitic clay is 17.48g, and carbon black is 23.85g.Final detection result: main thing is α '-Sialon and TiN mutually in the synthetic powder, contains a small amount of SiC and impurity in addition mutually.This diphase ceramic material volume density is 2.44g/cm
3, Vickers' hardness is 17GPa, and normal temperature ultimate compression strength is 427MPa, and resistivity at room temperature is about 5.60 * 10
6Ω cm belongs to semiconductor material.Behind 1300 ℃ of oxidation 3h, the unit surface oxidation weight gain is 13.24mg/cm
2
Example 7: (Ca, Mg) the first step of α '-Sialon diphase ceramic material and the processing step in second step and processing condition are with example 1 to produce TiN/.Different is that raw material is formulated as in the first step: getting titanium-containing blast furnace slag is 31.98g, and the silicon ash is 20.54g, and bauxitic clay is 24.41g, and carbon black is 23.07g.Final detection result: main thing is α '-Sialon and TiN mutually in the synthetic powder, contains a small amount of SiC and impurity in addition mutually.This diphase ceramic material volume density is 2.46g/cm
3, Vickers' hardness is 13GPa, and normal temperature ultimate compression strength is 435MPa, and resistivity at room temperature is about 3.65 * 10
6Ω cm belongs to semiconductor material.Behind 1300 ℃ of oxidation 3h, the unit surface oxidation weight gain is 14.87mg/cm
2
Example 8: (Ca, Mg) the first step of α '-Sialon diphase ceramic material and the processing step in second step and processing condition are with example 1 to produce TiN/.Different is that raw material is formulated as in the first step: titanium-containing blast furnace slag is 27.76g, and the silicon ash is 24.34g, and bauxitic clay is 21.16g, and carbon black is 26.74g.Final detection result: main thing is α '-Sialon and TiN mutually in the synthetic powder, contains a small amount of SiC and impurity in addition mutually.This diphase ceramic material volume density is 2.45g/cm
3, Vickers' hardness is 14GPa, and normal temperature ultimate compression strength is 532MPa, and resistivity at room temperature is about 4.46 * 10
6Ω cm belongs to semiconductor material.Behind 1300 ℃ of oxidation 3h, the unit surface oxidation weight gain is 15.02mg/cm
2
Example 9: (Ca, Mg) the first step of α '-Sialon diphase ceramic material and the processing step in second step and processing condition are with example 1 to produce TiN/.Different is that raw material is formulated as in the first step: titanium-containing blast furnace slag is 21.53g, and the silicon ash is 18.88g, and bauxitic clay is 16.41g, and carbon black is 43.18g.Final detection result: main thing is α '-Sialon and TiN mutually in the synthetic powder, contains a small amount of SiC and impurity in addition mutually.This diphase ceramic material volume density is 2.52g/cm
3, Vickers' hardness is 16GPa, and normal temperature ultimate compression strength is 431MPa, and resistivity at room temperature is about 2.95 * 10
6Ω cm belongs to semiconductor material.Behind 1300 ℃ of oxidation 3h, the unit surface oxidation weight gain is 14.15mg/cm
2
Claims (3)
1, a kind of utilize titanium-containing blast furnace slag to prepare TiN/ (Ca, Mg) method of α '-Sialon diphase ceramic material is characterized in that: with TiO
2Content is that 22～26% titanium-containing blast furnace slag is a main raw material, uses SiO
2Content is 82～90% silicon ash and Al
2O
3Content is 79～85% bauxitic clay adjustment composition, and carbon black is a reductive agent; Produce in two steps TiN/ (Ca, Mg) α '-Sialon diphase ceramic material:
The first step: synthetic TiN/ (Ca, Mg) α '-Sialon powder
(1) fragmentation: block titanium-containing blast furnace slag is carried out fragmentation, handle obtaining ground-slag then with the slag of sampling machine after to fragmentation;
(2) ball milling: the ground-slag bigger to above-mentioned granularity carries out fine grinding;
(3) sieve: sieve with the ground-slag of 200 purpose standard sieves after to above-mentioned fine grinding;
(4) magnetic separation: with magnet ground-slag is carried out magnetic separation, remove contained fe and ferromagnetic material in the ground-slag;
(5) batching: the chemical formula of selected synthetic α '-Sialon be (Ca, Mg)
xSi
12-3xAl
3xO
xN
16-x, x=0.3 in the formula～2.0 determine that the quality per distribution ratio of raw material is: titanium-containing blast furnace slag 5.22～31.98%, silicon ash 18.88～65.71%, bauxitic clay 3.66～24.41%, carbon black 23.06～43.19%;
(6) wet mixing: with prepared mixture is that medium is mixed into slip with the dehydrated alcohol, and the wet mixing time is 24 hours;
(7) drying: the slip after the wet mixing is put into baking oven in 60 ℃ of oven dry down;
(8) dried mixing: dried compound is done and was mixed 4 hours, and places moisture eliminator to preserve the gained blank;
(9) compression molding: the blank that will do after mixing carries out single shaft to compression moulding, and forming pressure is 25MPa, pressurize 1min;
(10) high temperature burns till: the blank of compression moulding is put into plumbago crucible, use MoSi
2High temperature resistance furnace heating is that 1450～1500 ℃, constant temperature time are that 6～10 hours, intensification and cooling rate are to feed continuously all the time in the stove under the flowing nitrogen condition that flow is 400～800ml/min in 3～5 ℃/min, the sintering process and carry out sintering at a normal atmosphere, firing temperature;
(11) burning-off carbon residue: with the above-mentioned TiN/ that sinters into (Ca, Mg) α '-Sialon powder places in the retort furnace, constant temperature was heat-treated in 6 hours in 580 ℃ of air, removed remaining uncombined carbon;
Second step: TiN/ (Ca, Mg) preparation of α '-Sialon diphase ceramic material
With the first step synthetic TiN/ (Ca, Mg) α '-Sialon powder and the addition of C aCO that accounts for raw material gross weight 10～15%
3Thorough mixing is even, is 200MPa at pressure, and single shaft is to compression molding, and pressurize 1min puts into plumbago crucible with these green compact then and imbeds by 60%Si
3N
4In the powder mix that+30%AlN+10%BN forms; place sintering oven, under the high pure nitrogen protection, carry out normal pressure, high temperature sintering; sintering temperature is 1600～1700 ℃; be incubated 1～2 hour; intensification is to take temperature increasing schedule stage by stage; heat-up rate is 5～30 ℃/min, and cooling rate is 30～40 ℃/min.
2, prepare TiN/ (Ca according to the described titanium-containing blast furnace slag that utilizes of claim 1, Mg) method of α '-Sialon diphase ceramic material, it is characterized in that high temperature sintering takes stage by stage that temperature increasing schedule is in second step: the speed with 25～30 ℃/min heats up earlier, when temperature reaches 1150 ℃, insulation 30min, after being warming up to 1400 ℃ with 25～30 ℃/min speed subsequently, the speed with 5～10 ℃/min rises to sintering temperature again.
3, according to claim 1 described utilize titanium-containing blast furnace slag to prepare TiN/ (Ca, the Mg) method of α '-Sialon diphase ceramic material is characterized in that the sintering oven that high temperature sintering adopts in second step is a vacuum carbon tube furnace.
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103278362A (en) * | 2013-06-03 | 2013-09-04 | 山东省冶金科学研究院 | Set of alum clay standard samples and preparation method thereof |
| US11691922B2 (en) | 2021-08-24 | 2023-07-04 | Industrial Technology Research Institute | Ceramic composite and method of preparing the same |
-
2005
- 2005-09-29 CN CN 200510047292 patent/CN1772703A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103278362A (en) * | 2013-06-03 | 2013-09-04 | 山东省冶金科学研究院 | Set of alum clay standard samples and preparation method thereof |
| CN103278362B (en) * | 2013-06-03 | 2015-07-15 | 山东省冶金科学研究院 | Set of alum clay standard samples and preparation method thereof |
| US11691922B2 (en) | 2021-08-24 | 2023-07-04 | Industrial Technology Research Institute | Ceramic composite and method of preparing the same |
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