CN102701725A - Honeycomb heating ceramic and preparation method thereof - Google Patents
Honeycomb heating ceramic and preparation method thereof Download PDFInfo
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- CN102701725A CN102701725A CN2012102027940A CN201210202794A CN102701725A CN 102701725 A CN102701725 A CN 102701725A CN 2012102027940 A CN2012102027940 A CN 2012102027940A CN 201210202794 A CN201210202794 A CN 201210202794A CN 102701725 A CN102701725 A CN 102701725A
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Abstract
The invention discloses a honeycomb heating ceramic and a preparation method thereof. The honeycomb heating ceramic is prepared from mixed ceramic powder comprising the following components by molar percentage: 96% of MgAl2O4, 1% to 3% of SiO2 and 3% to 1% of TiO2. Through the study on sintering temperature and holding time in the process conditions of preparation of the honeycomb heating ceramic, when the sintering temperature is 1300 to 1600 DEG C, and the holding time is 1 to 5h, the problems that the traditional honeycomb heating ceramic has higher room temperature resistivity and lower density and hardness can be effectively solved; and when the sintering temperature is 1600 DEG C, and the holding time is 2h, the prepared honeycomb ceramic has maximum density and microhardness which are respectively 86. 0% and 289.1HV, and has minimum room temperature resistivity of 6.4 *10<4 >omega m.
Description
Technical field
The present invention relates to cellular heating pottery and preparation method thereof, belong to the energy-conserving and environment-protective technical field.
Background technology
The hole shape of ceramic honeycomb material is a regular hexagon, is a kind of stupalith extremely similar with the nest of honey.Honey-combed belongs to a kind of relatively particular structural in the ceramic foam, be the discontinuous material of a kind of porous, and the sectional area of entity part is very little, so the density of ceramic honeycomb is smaller, is a kind of very light material.
Ceramic honeycomb more and more receives people's attention as a kind of new ceramic material.In recent years, along with Development of Preparation Technology, its range of application constantly enlarges, and application level also improves constantly.Compare with traditional particulate state ceramic monolith, the vesicular cellular structure ceramic carrier have pressure fall little, geometric jacquard patterning unit surface is big, extended range is short, help the entering of reactant and the discharge of resultant, and the advantages such as volume that can dwindle reactor drum.Therefore ceramic honeycomb is specially adapted to the aspects such as purification, heat storage and ir radiation burner plate of vehicle exhaust processing, flue gas.
Continuous development along with science and technology; Cellular heating pottery has appearred again in early 1990s; Compare with traditional heat storage, great variety-develop into ceramic bead from original checker brick has taken place in its regenerator, develops into ceramic honeycomb again; The specific surface area of regenerator is sharply increased, volume obviously reduces, shorten turnaround time greatly, heat exchange property is greatly improved, pollutant discharge amount is also far below the emission standard of Environmental Protection Agency regulation.But at present the cellular heating pottery of made still exist room temperature resistivity greatly, density and the less shortcoming of hardness, need further improve.The applicant retrieves Chinese patent gazette, does not find the report of the patented claim of the ceramic aspect of cellular heating as yet.
Summary of the invention
The objective of the invention is to, a kind of cellular heating pottery and preparation method thereof is provided, it can effectively solve the problem that exists in the prior art, and the room temperature resistivity of particularly cellular heating pottery is big, density and hardness problem of smaller.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of cellular heating pottery, and it is prepared from the hybrid ceramic powder; Described hybrid ceramic powder calculates the MgAl by 96% according to molar percentage
2O
4, 1%～3% SiO
2With 3%～1% TiO
2Form.
Concrete, it is prepared from the hybrid ceramic powder; Described hybrid ceramic powder calculates the MgAl by 96% according to molar percentage
2O
4, 2% SiO
2With 2% TiO
2Form.
Described MgAl
2O
4By mol ratio is the Al of 1:1
2O
3Reaction generates with MgO.
Concrete, described Al
2O
3Be a-Al
2O
3
A kind of preparation method of aforesaid cellular heating pottery will be by MgAl
2O
4, SiO
2And TiO
2The hybrid ceramic powder of forming grinds, ball milling 8～24h behind the interpolation dispersion agent, and ceramic powder material must generate heat; The ceramic powder material that should generate heat carries out drying, pugging, old, and utilizes extruder for shaping, gets base substrate; Base substrate is carried out drying and sintering processes; Described sintering processes specifically comprises: will discharge and be incubated 30min after dry base substrate behind the moisture is warming up to 150 ℃ with the speed of 5 ℃/min at ambient temperature; Speed with 5 ℃/min is warming up to 850 ℃ of insulation 120min again; After being warming up to 1300～1600 ℃ of insulation 1～5h with the speed of 10 ℃/min again, base substrate is cooled to below 50 ℃, cellular heating ceramics sample; On cellular heating ceramics sample, prepare electrode, get cellular heating pottery.
Concrete, will be by MgAl
2O
4, SiO
2And TiO
2The hybrid ceramic powder of forming grinds, ball milling 20h behind the interpolation dispersion agent, and ceramic powder material must generate heat; The ceramic powder material that should generate heat carries out drying, pugging, old, and utilizes extruder for shaping, gets base substrate; Base substrate is carried out drying and sintering processes; Described sintering processes specifically comprises: will discharge and be incubated 30min after dry base substrate behind the moisture is warming up to 150 ℃ with the speed of 5 ℃/min at ambient temperature; Speed with 5 ℃/min is warming up to 850 ℃ of insulation 120min again; After being warming up to 1600 ℃ of insulation 2h with the speed of 10 ℃/min again, base substrate is cooled to below 50 ℃, cellular heating ceramics sample; On cellular heating ceramics sample, prepare electrode, get cellular heating pottery.
In the preceding method, described MgAl
2O
4, be the Al of 1:1 by mol ratio
2O
3Mix with MgO, behind the ball milling, put into resistance furnace and be warming up to 1200 ℃ and be incubated the 120min sintering and promptly get.
In the preceding method, at Al
2O
3Before MgO mixes, to Al
2O
3Calcine, thereby make γ-Al
2O
3All be converted into the a-Al that structure is tight, activity is low, all have good chemicalstability in each temperature province
2O
3, reduce later stage base substrate volumetric shrinkage, simultaneously can despumation Na in calcination process
2O reaches the purpose that improves material purity.
In order to verify the exercising result of aforesaid method to cellular heating pottery, the applicant has carried out series of experimental research, and is specific as follows:
1, the ball milling time is to the influence of diameter of particle distribution
Formulation data weighing powder according to the method described above with its thorough mixing, adds a small amount of absolute ethyl alcohol as dispersion agent; Put into aluminum oxide ball milling jar after mixing; Agate ball and powder ratio are 1:10, and drum's speed of rotation is 720 commentaries on classics/min, and powder is carried out 8～24h ball milling.Along with the increase of ball milling time, the reducing of powder particle size is tending towards slowly, and grinding efficiency can reduce, and long-time ball milling will consume more electric energy.Therefore, should under the prerequisite that satisfies the diameter of particle requirement, shorten the ball milling time as far as possible.This experiment adopts JL-1155 type laser particle size distribution tests appearance to measure the diameter of particle of different ball millings after the time, the powder median size that the different ball milling times are corresponding and distribute as shown in table 1.Fig. 1 is the relation of different ball milling times and powder median size.
Table 1
| Sample number into spectrum | I | II | III | IV | V |
| Milling time (h) | 8 | 12 | 16 | 20 | 24 |
| Median size (μ m) | 1.28 | 1.16 | 1.15 | 1.01 | 1.00 |
| Accumulate 50% particle diameter (μ m) | 1.12 | 0.98 | 0.93 | 0.90 | 0.90 |
By table 1 and combine Fig. 1 to find out, mixed powder is through behind the ball milling of certain hour, and its granularity and size distribution significantly improve.The ball milling time is long more, and the powder granularity that obtains is more little, and the effect of ball milling is also good more, and at 8～12h of beginning, diameter of particle reduces comparatively fast.Particle diameter keeps 0.9 μ m constant basically after the ball milling time reaches 20h.Fig. 2 is different ball milling accumulated time 50% size distribution figure, and it is wide than the diameter of particle distribution of ball milling 24h to know that by Fig. 2 the diameter of particle of ball milling 20h distributes.
Fig. 3, Fig. 4 are respectively the powder SEM picture behind ball milling 20h and the 24h, and the mixed powder pattern behind ball milling 20h and 24h can find out that the distribution of mixed powder is more even behind the ball milling 20h; And ball milling 24h, mixed powder begins to occur agglomeration.And the ball milling time is long more, and the energy that is consumed is many more, and therefore, after taking all factors into consideration, choosing the powder ball milling time is 20h.
2, different sintering temperatures are to the influence of microstructure
With Al
2O
3With MgO in molar ratio 1:1 mix, behind the ball milling 20h at 1200 ℃ of sintering and MgAl
2O
4The basic batching mol ratio of cellular heating pottery is MgAl
2O
4: SiO
2: TiO
2=96:2:2 through batching, mixing → ball milling → drying → pugging, old → extrusion moulding → drying process, makes base substrate.In order to explore 96MgAl
2O
4-2SiO
2-2TiO
2The optimal sintering temperature of cellular heating pottery test used sintering temperature and is respectively 1300 ℃, 1400 ℃, 1500 ℃ and 1600 ℃ (this breadboard chamber type electric resistance furnace theory maximum heating temperature is 1650 ℃), and soaking time is 2h.
The cellular heating ceramics sample knock size of sintering gained under the differing temps is about 0.5 * 0.5mm
2～1.0 * 1.0mm
2Fritter; After respectively 1～No. 4 sample fritter being cleaned 10min with the JK-2200 Ultrasonic Cleaners; Place microwave oven, 110 ℃ leave standstill 10min and carry out drying, with the gold-plated film device of JEOL JFC-1600 type metal spraying Processing of Preparation conductive layer are carried out on the surface; Use its microstructure of JSE-6490LV surface sweeping electron microscopic observation then, the tissue topography of cellular heating pottery such as Fig. 5, Fig. 6, Fig. 7, shown in Figure 8 under the differing temps.As can be seen from the figure, along with the increase of sintering temperature, grain-size becomes greatly gradually, and intergranule forms tight contact gradually, and bore hole size and pore quantity slowly reduce, and have improved the density of sample.In 1300 ℃ of agglomerating sample topography Fig. 5, just be deposited in simply together between the powder granule, there is tangible hole between the particle; Sample structure is more open; Sintering does not take place in powder basically, explains that sintering temperature does not reach the sintering requirement, needs to continue to improve ceramic sintering temperature; When sintering temperature is 1400 ℃; In sample topography Fig. 6, having observed a large amount of small grains exists; But the grain growth degree is not obvious, and most of grain-size is 0.3～0.8 μ m, and intergranule exists a large amount of large size hole and void distribution inhomogeneous; Explain that sintering temperature is on the low side, the sample underburnt; When sintering temperature is increased to 1500 ℃; Have clear improvement when from sample topography Fig. 7, observing the grain growth situation than 1400 ℃, grain-size is 0.8～1.2 μ m, and grain size distribution is more even; Crystal grain and intergranule are in contact with one another, and pore quantity obviously reduces; When sintering temperature is increased to 1600 ℃, from the shape appearance figure 8 of sample, see that grain growth is apparent in view; Grain-size is 1.0～2.0 μ m; Grain size is evenly distributed, and crystal grain forms good the contact with intergranule, has only the small size hole of minute quantity to remain in the pottery.Explain that 1600 ℃ are satisfied 96MgAl basically
2O
4-2SiO
2-2TiO
2The sintering requirement of cellular heating pottery.With 96MgAl
2O
4-2SiO
2-2TiO
2The sintering temperature of cellular heating pottery is confirmed as 1600 ℃.In subsequent experimental, can eliminate the remaining hole that lacked through the proper extension soaking time, improve ceramic microstructure.
3, different sintering temperatures are to the influence of density
For general solid material,, just can pass through formula as long as know its quality and volume:
ρ=m/v （1）
The density of measure solid.The quality of object can directly be measured through Libra and get; For object in irregular shape; Be difficult to directly measure its volume,, need solve by buoyancy method for the density of this type irregular-shaped objects; Promptly utilize Archimedes' principle to measure the density of out-of-shape object, like the measuring apparatus of Fig. 9 for designing voluntarily according to Archimedes' principle.
If the density of testee is greater than known density of liquid, adopt " immersion method ", promptly object be immersed in buoyancy suffered in the liquid can be by the actual mass m of object
1With apparent weight m
2Difference obtain (" apparent weight " refers to that object is immersed in gravity measured in the liquid), calculate object volume by Archimedes' principle again:
V=(m
1-m
2)/ρg （2）
Then the density of object is:
ρ
Thing=m
1ρ
Liquid/ (m
1-m
2) (3)
Through aforesaid method, record 96MgAl under different sintering temperatures respectively
2O
4-2SiO
2-2TiO
2The density of cellular heating ceramics sample, shown in figure 10.
Data by among Figure 10 show that along with the increase of sintering temperature, the density of sample increases gradually.When sintering temperature was 1300 ℃, sintering did not take place in powder granule basically, and sample structure is more open, has a large amount of holes between particle, caused the density of sample very little; When sintering temperature was 1400 ℃, though there are many small grains in the sample, crystal grain was not also grown up, and had more large size hole in the sample, so density increases slowly; When sintering temperature was brought up to 1500 ℃, crystal grain took place obviously to grow up, and grain-size is more even; Crystal grain and intergranule are in contact with one another, and large size hole quantity obviously reduces, and part small size pore remains in the sample; Make the density of sample that increase arranged slightly, reach 82.4%; When further sintering temperature being brought up to 1600 ℃, the crystal grain of evenly growing up closely contacts with intergranule, but still has minute quantity small size pore to remain in the sample, and the density of sample reaches 86.0% under this temperature.
4, different sintering temperatures are to the influence of hardness
Respectively with 1300 ℃, 1400 ℃, 1500 ℃ and 1600 ℃ of insulation 2h solid state sintering gained 96MgAl
2O
4-2SiO
2-2TiO
2Cellular heating ceramics sample is broken into pieces, chooses the ceramics that size is about 4mm * 4mm～8mm * 8mm and on P-2 type mounting press, inlays appearance with polyvinyl chloride powder, obtains being of a size of the right cylinder of Ф 10mm * 13mm, uses 1～6 successively
#Abrasive paper for metallograph polishes the sample flour milling, and the polishing principle is identical with test button mill method.After water washes down flour milling; With particle diameter is that the diamond paste of 10 μ m is evenly coated on the polishing cloth; Be contained in that the polished face to sample carries out mechanical polishing on the polishing machine that model is PG-2D, make polished face become smooth mirror surface, after with deionized water polished surface being washed down; Dip in medical cotton pellet and to get absolute ethyl alcohol wiping polished surface gently, with blower polished surface is dried up again.Using concentration is that 15% hydrofluoric acid is as corrosive fluid; Utilize the Olympus metallography microscope sem observation microstructure of model for GX51; Hardness measurement uses HV-1000 type Vickers hardness tester that the sample polished surface is got a little; Pressure is 300N, and the dwell time is 20s, utilizes the diagonal lines rule to calculate the hardness value of sample respectively.Shown in figure 11.
As can beappreciated from fig. 11,96MgAl
2O
4-2SiO
2-2TiO
2The hardness value of cellular heating ceramics sample increases along with the rising of sintering temperature.When sintering temperature was 1300 ℃, sintering did not take place in powder, and the sample hardness value is merely 191.2HV; Along with sintering temperature increases, crystal grain is grown up gradually, and even grain size distributes; When sintering temperature was 1500 ℃, grain growth was obvious, and crystal grain forms good the contact with intergranule; Hole quantity reduces; The hardness value of sample increases very fast, and the hardness value of sample is maximum when sintering temperature is 1600 ℃, and peak is 289.1HV.
5, different sintering temperatures are to the influence of room temperature resistivity
Respectively at 1300 ℃, 1400 ℃, 1500 ℃ and 1600 ℃ of 96MgAl that are incubated 2h solid state sintering gained
2O
4-2SiO
2-2TiO
2The two ends brush silver slurry of cellular heating ceramics sample is dried under 110 ℃ condition, places SX3-8-10 molding box formula resistance furnace behind 850 ℃ of sintering 2h, cools to the furnace below 100 ℃, makes electrode.Under the room temperature, adopt the resistance value of pH/Cond 3400i type hand-held resistance meter measure sample, for ceramics sample, the relation of resistance and resistivity is:
（4）
Wherein, R: resistance value (Ω); ρ: resistivity (Ω .m); T (probe temperature): 25 ℃; L (specimen length): 1.2 * 10
-2M; W (sample weight): 2.5 * 10
-3Kg; D (distance between the current potential point of contact): 10
-3M; D (proportion of copper): (8.89 * 10
3Kg/m
3); A: temperature correction facotor (1/ ℃), a=0.00377; W: the thickness of material (m).
Table 2 is respectively at 1300 ℃, 1400 ℃, 1500 ℃ and the 1600 ℃ room temperature resistivities that are incubated 2h solid state sintering gained samples.
Can find out that by table 2 along with the increase of sintering temperature, the room temperature resistivity of sample reduces gradually, when sintering temperature when 1300 ℃ are upgraded to 1600 ℃, the room temperature resistivity of sample is from 1.6 * 10
8Ω .m is reduced to 6.4 * 10
4Ω .m, the range of decrease is big by 10
4The order of magnitude.Therefore, the optimal sintering temperature of cellular heating pottery is 1600 ℃.
Table 2
| | 1 | 2 | 3 | 4 |
| Sintering temperature (℃) | 1300 | 1400 | 1500 | 1600 |
| Room temperature resistivity (Ω .m) | 1.6 * 10 8 | 3.4 * 10 7 | 2.6 * 10 5 | 6.4 * 10 4 |
Compared with prior art; The present invention is through studying sintering temperature and hold-time in the processing condition that prepare cellular heating pottery; When sintering temperature is 1300～1600 ℃; Insulation is during 1～5h, and the room temperature resistivity that can effectively improve existing cellular heating pottery is big, density and hardness problem of smaller; And when sintering temperature is 1600 ℃, insulation is during 2h, and density, the microhardness of the cellular heating pottery for preparing reach maximum, and its peak is respectively 86.0% and 289.1HV, makes room temperature resistivity reach minimum simultaneously, and its minimum value is 6.4 * 10
4Ω .m.In addition, the present invention studied and screens the ball milling time of hybrid ceramic powder, when ball milling 20h, can obtain of uniform size, that the diameter of particle distribution is wider and the powder granule particle diameter minimum, and its particle diameter minimum value is 0.9 μ m.The present invention has effectively solved the problem that exists in the prior art.
Description of drawings:
Fig. 1 is the synoptic diagram that concerns of different ball milling times and powder median size;
Fig. 2 is the distribution plan of different ball milling accumulated time 50% particle diameters;
Fig. 3 is the powder SEM picture behind the ball milling 20h;
Fig. 4 is the powder SEM picture behind the ball milling 24h;
Fig. 5 is the figure of tissue topography of cellular heating pottery under 1300 ℃ sintering temperature;
Fig. 6 is the figure of tissue topography of cellular heating pottery under 1400 ℃ sintering temperature;
Fig. 7 is the figure of tissue topography of cellular heating pottery under 1500 ℃ sintering temperature;
Fig. 8 is the figure of tissue topography of cellular heating pottery under 1600 ℃ sintering temperature;
Fig. 9 is the measuring apparatus figure according to Archimedes' principle designed;
Figure 10 is the density synoptic diagram of cellular heating pottery under different sintering temperatures;
Figure 11 is the hardness value synoptic diagram of cellular heating pottery under different sintering temperatures.
Description of drawings:
The 1-Libra; The 2-sample; 3-liquid; The container in 4-carry potential overflow hole; The 5-counterweight; The liquid that 6-overflows.
Embodiment
Embodiment 1: a kind of cellular heating pottery, and it is prepared from the hybrid ceramic powder; Described hybrid ceramic powder calculates the MgAl by 96% according to molar percentage
2O
4, 2% SiO
2With 2% TiO
2Form.Described MgAl
2O
4By mol ratio is the Al of 1:1
2O
3Reaction generates with MgO.Described Al
2O
3Be a-Al
2O
3
A kind of preparation method of above-mentioned cellular heating pottery comprises: get Al
2O
3After calcining, be the Al of 1:1 with mol ratio
2O
3Behind MgO mixing, ball milling, put into resistance furnace and be warming up to 1200 ℃ of insulation 120min sintering, get MgAl
2O
4Phase; Calculate according to molar percentage: MgAl 96%
2O
4, 2% SiO
2, 2% TiO
2Mix, grind, add dispersion agent ball milling 20h, obtain the ceramic powder material that generates heat; This heating ceramic powder material is put into beaker and placed 110 ℃ loft drier 4h, obtain dry powder; The Z 150PH of getting dry powder total mass 15% is poured in the above-mentioned beaker that fills dry powder; Stir; Powder is mixed with Z 150PH; Pour into again in the stirrer and take out behind the stirring 30min, place thick pug mill to carry out 5 times thick puggings, mixed and have the polycomponent mixing blank of processability; To mix the old 24h of blank, utilize the plunger type extruder extrusion moulding, obtain base substrate; The heating base substrate is discharged the laggard capable blank sintering of moisture and is handled; Described sintering processes specifically comprises: will discharge and be incubated 30min after dry base substrate behind the moisture is warming up to 150 ℃ with the speed of 5 ℃/min at ambient temperature; Speed with 5 ℃/min is warming up to 850 ℃ of insulation 120min again; After being warming up to 1600 ℃ of insulation 2h with the speed of 10 ℃/min again, base substrate is cooled to below 50 ℃, obtains cellular heating ceramics sample; When sample is cooled to room temperature; The brush silver slurry at the two ends of cellular heating ceramics sample puts it in 110 ℃ the baking oven and leaves standstill 30min, takes out and be placed in the box-type furnace then; Speed with 5 ℃/min is warming up to 200 ℃ of insulation 60min; Speed with 10 ℃/min is warming up to 850 ℃ of insulation 120min again, and cooling is come out of the stove below 100 ℃, promptly gets cellular heating pottery.Wherein, a-Al
2O
3Can be provided by the extremely prosperous chemical industry in Shanghai ltd, its purity is 99%; TiO
2Can be provided by Tianjin section close europeanized reagent development centre, its purity is 99%; MgO can be provided by Tianjin section close europeanized reagent development centre, and its purity is 98%; Z 150PH can help chemical industry ltd to provide by Shanghai more, its purity>=99.99%.
Embodiment 2: a kind of cellular heating pottery, to calculate according to molar percentage, and it is by 96% MgAl
2O
4, 3% SiO
2With 1% TiO
2Be mixed with and form.Described MgAl
2O
4By mol ratio is the Al of 1:1
2O
3Reaction generates with MgO.A kind of preparation method of above-mentioned cellular heating pottery comprises: be the Al of 1:1 with mol ratio
2O
3Behind MgO mixing, ball milling, put into resistance furnace and be warming up to 1200 ℃ of insulation 120min sintering, get MgAl
2O
4Phase; Calculate according to molar percentage: MgAl 96%
2O
4, 3% SiO
2, 1% TiO
2Mix, grind, add dispersion agent ball milling 24h, obtain the ceramic powder material that generates heat; This heating ceramic powder material is put into beaker and placed 110 ℃ loft drier 4h, obtain dry powder; The Z 150PH of getting dry powder total mass 15% is poured in the above-mentioned beaker that fills dry powder; Stir; Powder is mixed with Z 150PH; Pour into again in the stirrer and take out behind the stirring 30min, place thick pug mill to carry out 5 times thick puggings, mixed and have the polycomponent mixing blank of processability; To mix the old 24h of blank, utilize the plunger type extruder extrusion moulding, obtain base substrate; The heating base substrate is discharged the laggard capable blank sintering of moisture and is handled; Described sintering processes specifically comprises: will discharge and be incubated 30min after dry base substrate behind the moisture is warming up to 150 ℃ with the speed of 5 ℃/min at ambient temperature; Speed with 5 ℃/min is warming up to 850 ℃ of insulation 120min again; After being warming up to 1600 ℃ of insulation 5h with the speed of 10 ℃/min again, base substrate is cooled to below 50 ℃, obtains cellular heating ceramics sample; When sample is cooled to room temperature; The brush silver slurry at the two ends of cellular heating ceramics sample puts it in 110 ℃ the baking oven and leaves standstill 30min, takes out and be placed in the box-type furnace then; Speed with 5 ℃/min is warming up to 200 ℃ of insulation 60min; Speed with 10 ℃/min is warming up to 850 ℃ of insulation 120min again, and cooling is come out of the stove below 100 ℃, promptly gets cellular heating pottery.
Embodiment 3: a kind of cellular heating pottery, to calculate according to molar percentage, and it is by 96% MgAl
2O
4, 1% SiO
2With 3% TiO
2Be mixed with and form.Described MgAl
2O
4By mol ratio is the Al of 1:1
2O
3Reaction generates with MgO.Described Al
2O
3Be a-Al
2O
3
A kind of preparation method of above-mentioned cellular heating pottery comprises: be the Al of 1:1 with mol ratio
2O
3Behind MgO mixing, ball milling, put into resistance furnace and be warming up to 1200 ℃ of insulation 120min sintering, get MgAl
2O
4Phase; Calculate according to molar percentage: MgAl 96%
2O
4, 1% SiO
2, 3% TiO
2Mix, grind, add dispersion agent ball milling 8h, obtain the ceramic powder material that generates heat; This heating ceramic powder material is put into beaker and placed 110 ℃ loft drier 4h, obtain dry powder; The Z 150PH of getting dry powder total mass 15% is poured in the above-mentioned beaker that fills dry powder; Stir; Powder is mixed with Z 150PH; Pour into again in the stirrer and take out behind the stirring 30min, place thick pug mill to carry out 5 times thick puggings, mixed and have the polycomponent mixing blank of processability; To mix the old 24h of blank, utilize the plunger type extruder extrusion moulding, obtain base substrate; The heating base substrate is discharged the laggard capable blank sintering of moisture and is handled; Described sintering processes specifically comprises: will discharge and be incubated 30min after dry base substrate behind the moisture is warming up to 150 ℃ with the speed of 5 ℃/min at ambient temperature; Speed with 5 ℃/min is warming up to 850 ℃ of insulation 120min again; After being warming up to 1300 ℃ of insulation 1h with the speed of 10 ℃/min again, base substrate is cooled to below 50 ℃, obtains cellular heating ceramics sample; When sample is cooled to room temperature; The brush silver slurry at the two ends of cellular heating ceramics sample puts it in 110 ℃ the baking oven and leaves standstill 30min, takes out and be placed in the box-type furnace then; Speed with 5 ℃/min is warming up to 200 ℃ of insulation 60min; Speed with 10 ℃/min is warming up to 850 ℃ of insulation 120min again, and cooling is come out of the stove below 100 ℃, promptly gets cellular heating pottery.
Claims (8)
1. a cellular heating is ceramic, and it is characterized in that: it is prepared from the hybrid ceramic powder; Described hybrid ceramic powder calculates the MgAl by 96% according to molar percentage
2O
4, 1%～3% SiO
2With 3%～1% TiO
2Form.
2. cellular heating pottery according to claim 1 is characterized in that it is prepared from the hybrid ceramic powder; Described hybrid ceramic powder calculates the MgAl by 96% according to molar percentage
2O
4, 2% SiO
2With 2% TiO
2Form.
3. cellular heating pottery according to claim 1 and 2 is characterized in that described MgAl
2O
4By mol ratio is the Al of 1:1
2O
3Reaction generates with MgO.
4. cellular heating pottery according to claim 3 is characterized in that described Al
2O
3Be a-Al
2O
3
5. a kind of preparation method of the arbitrary said cellular heating pottery of claim 1～4 is characterized in that: will be by MgAl
2O
4, SiO
2And TiO
2The hybrid ceramic powder of forming grinds, ball milling 8～24h behind the interpolation dispersion agent, and ceramic powder material must generate heat; The ceramic powder material that should generate heat carries out drying, pugging, old, and utilizes extruder for shaping, gets base substrate; Base substrate is carried out drying and sintering processes; Described sintering processes specifically comprises: will discharge and be incubated 30min after dry base substrate behind the moisture is warming up to 150 ℃ with the speed of 5 ℃/min at ambient temperature; Speed with 5 ℃/min is warming up to 850 ℃ of insulation 120min again; After being warming up to 1300～1600 ℃ of insulation 1～5h with the speed of 10 ℃/min again, base substrate is cooled to below 50 ℃, cellular heating ceramics sample; On cellular heating ceramics sample, prepare electrode, get cellular heating pottery.
6. the preparation method of cellular heating pottery according to claim 5 is characterized in that: will be by MgAl
2O
4, SiO
2And TiO
2The hybrid ceramic powder of forming grinds, ball milling 20h behind the interpolation dispersion agent, and ceramic powder material must generate heat; The ceramic powder material that should generate heat carries out drying, pugging, old, and utilizes extruder for shaping, gets base substrate; Base substrate is carried out drying and sintering processes; Described sintering processes specifically comprises: will discharge and be incubated 30min after dry base substrate behind the moisture is warming up to 150 ℃ with the speed of 5 ℃/min at ambient temperature; Speed with 5 ℃/min is warming up to 850 ℃ of insulation 120min again; After being warming up to 1600 ℃ of insulation 2h with the speed of 10 ℃/min again, base substrate is cooled to below 50 ℃, cellular heating ceramics sample; On cellular heating ceramics sample, prepare electrode, get cellular heating pottery.
7. according to the preparation method of claim 5 or 6 described cellular heating potteries, it is characterized in that: described MgAl
2O
4, be the Al of 1:1 by mol ratio
2O
3Mix with MgO, behind the ball milling, put into resistance furnace and be warming up to 1200 ℃ and be incubated the 120min sintering and promptly get.
8. the preparation method of cellular heating pottery according to claim 7 is characterized in that: at Al
2O
3Before MgO mixes, to Al
2O
3Calcine.
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| CN112268476A (en) * | 2020-10-13 | 2021-01-26 | 鲁励成 | High temperature resistant heat storage and release insulation box |
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