CN104140255B - A kind of method utilizing tricalcium phosphate to prepare high tenacity pottery - Google Patents
A kind of method utilizing tricalcium phosphate to prepare high tenacity pottery Download PDFInfo
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- CN104140255B CN104140255B CN201410371323.1A CN201410371323A CN104140255B CN 104140255 B CN104140255 B CN 104140255B CN 201410371323 A CN201410371323 A CN 201410371323A CN 104140255 B CN104140255 B CN 104140255B
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Abstract
The invention belongs to ceramic industry field, disclose a kind of method utilizing tricalcium phosphate to prepare high tenacity pottery.It is as follows that described method comprises step: by weight percentage, and by the tricalcium phosphate of 5% ~ 15% and 85% ~ 95% ceramic batch, to pulverize mix grinding even for the mode of ball milling in a wet process, drying and grinding into powder, dry-pressing formed obtained ceramic green, green compact burn till in kiln, obtained high tenacity pottery.The high tenacity ceramics sample prepared of the method with acicular mullite and lime feldspar for principal crystalline phase, cristobalite is paracrystalline phase, Si-O system is Binder Phase with P-O system compound glass mutually, thermal expansivity between this structure crystalline phase, between crystalline phase and glassy phase mates more, effectively can reduce the generation of tiny crack in ceramic firing process, increase substantially the toughness of ceramic product.
Description
Technical field
The invention belongs to ceramic industry field, relate to silicate industry ceramic preparation, be specifically related to a kind of method utilizing tricalcium phosphate to prepare high tenacity pottery.
Background technology
China is Production of Ceramics big country, and traditional ceramics is very flourishing, and output occupies first place in the world for many years.Current ceramic industry facing challenges mainly contains: Production of Ceramics energy consumption is larger; The resistance to impact shock of product is on the low side, and toughness is poor; The raw material of high-quality reduces day by day.In traditional clay-quartz-feldspar system, porcelain body is mainly with cristobalite (α-SiO
2), mullite (Al
6si
2o
13) be principal crystalline phase, Si-O glass is Binder Phase.Wherein cristobalite particle size is generally between several microns to tens microns, and mullite is mainly flakey and granular primary mullite, and cristobalite thermal expansivity is 11 × 10
-6/ DEG C, mullite thermal expansivity is 5.7 × 10
-6/ DEG C, the thermal expansivity of feldspathic glass phase is 5.3 ~ 5.8 × 10
-6/ DEG C, the thermal expansivity of visible cristobalite and mullite, feldspathic glass differs greatly, and in sintering process, because each contraction mutually is not mated, easily causes product to produce tiny crack, reduces intensity and the thermostability of ceramic product, affect quality product.
With the lime feldspar (CaAl that calcium, aluminium, silicon, oxygen are main composition
2si
2o
8) thermal expansivity is 4.9 ~ 5.5 × 10
-6/ DEG C, all very close mutually with mullite crystalline phase and feldspathic glass, replace the principal crystalline phase of part cristobalite as pottery using lime feldspar, contribute to reducing the thermal expansion coefficient difference between principal crystalline phase, between principal crystalline phase and glassy phase.Simultaneously lime feldspar is needle-like pattern, and the having to be beneficial to of needle-like principal crystalline phase improves microstructure of ceramics, enhances product performance, particularly toughness.
Utilize lime feldspar toughening ceramic early to have research, but its research is mainly partial to, according to crystal chemistry composition design composition of raw materials, be mainly SiO
2, Al
2o
3and CaCO
3deng, synthesis obtains single lime feldspar/mullite compound phase material, and synthesis temperature is generally more than 1400 DEG C, and complex process.
The mode that calcium normally joins in ceramic batch with calcium salt is introduced, and the kind of calcium salt is a lot, wherein takes the mode of calcium phosphate, while introducing calcium, also introduces phosphorus.Similar with silicon, at high temperature phosphorus also easily forms glassy phase, and Si-O system and P-O system compound glass phase thermal expansivity are 5.6 ~ 6.2 × 10
-6/ DEG C, mate all very much with feldspathic glass phase, mullite crystalline phase and lime feldspar crystalline phase, disadvantageous effect can not be caused to product performance.
Tricalcium phosphate exists with white crystal or unformed powder, is mainly used in and prepares foodstuff additive, biological ceramics, Bone China, staining agent, fluorescent material etc.
Summary of the invention
The problem such as high for firing temperature in current ceramic industry, high-quality feedstocks reduces day by day, product performance have much room for improvement, the object of the present invention is to provide a kind of method utilizing tricalcium phosphate to prepare high tenacity pottery, described method can improve the toughness of ceramic product.
Object of the present invention is achieved through the following technical solutions:
Utilize tricalcium phosphate to prepare a method for high tenacity pottery, comprise the steps:
(1) by tricalcium phosphate and ceramic batch mixing, the mode mix grinding of ball milling evenly obtains slurry in a wet process;
(2) step (1) gained slurry is sieved, dries, grind into powder, after sieve, dry-pressing formed, pressurize, obtained ceramic green;
(3) described ceramic green is burnt till in kiln, obtained high tenacity pottery.
Prepare in the method for high tenacity pottery at the above-mentioned tricalcium phosphate that utilizes:
Preferably, the incorporation of step (1) described tricalcium phosphate accounts for 5% ~ 15% of tricalcium phosphate and ceramic batch total mass;
Preferably, the composition of step (1) described ceramic batch and mass percentage are: SiO
2: 65.14% ~ 70.27%, Al
2o
3: 18.01% ~ 22.56%, K
2o:1.68% ~ 2.24%, Na
2o:0.4% ~ 0.97%, MgO:0.13% ~ 0.48%, Fe
2o
3: 0.37% ~ 0.82%, CaO:0.15% ~ 0.52%, P
2o
5: 0.10% ~ 0.23%, burn mistake: 7.61% ~ 8.44%;
Preferably, the temperature of step (2) described oven dry is 100 DEG C;
Preferably, the pressure of step (2) described pressurize is 15MPa, and the dwell time is 1 minute;
Preferably, the temperature that step (3) described ceramic green burns till is 1180 ~ 1280 DEG C; Preferred, the temperature that step (3) described ceramic green burns till is 1200 ~ 1240 DEG C;
Preferably, the soaking time that step (3) described ceramic green burns till is 60 ~ 90 minutes; Preferred, the soaking time that step (3) described ceramic green burns till is 70 ~ 80 minutes.
Principle of the present invention:
Tricalcium phosphate is incorporated in ceramic batch by the present invention, on the one hand as the source of calcareous element, lime feldspar is generated in sintering process, the introducing of calcareous element simultaneously, the temperature that in ceramic firing process, liquid phase occurs can be reduced, change the physico-chemical property of high-temperature fusant, contribute to quartz and flakey, granular primary mullite melting, and then generate the secondary mullite of needle-like, thus excellent crystalline structure can be formed at a lower temperature: more acicular mullite and lime feldspar crystal, a small amount of cristobalite; On the other hand as the source of phosphoric, generate Si-O system and P-O system compound glass phase in the product, the melt temperature of quartz in P-O system glass be low relative to Si-O system glass 50 DEG C ~ and 200 DEG C, the melting of cristobalite and secondary mullite, anorthitic generation can be accelerated further.Final formation with acicular mullite and lime feldspar be principal crystalline phase, the microstructure of Si-O system and P-O system compound glass phase, between each phase, thermal expansivity matches, the generation of micro-flaw in ceramic firing process can be reduced, significantly improve toughness and the intensity of ceramic product.
The present invention has following advantage and effect relative to prior art:
(1) the present invention utilizes tricalcium phosphate to provide calcium and phosphorus, generates lime feldspar and Si-O system and P-O system compound glass phase, can increase substantially the toughness of ceramic product in ceramic firing process.The introducing of calcareous element reduces the temperature that in sintering process, liquid phase occurs, changes the physico-chemical property of high-temperature liquid-phase, accelerates the melting of quartz and the generation of needle-like secondary mullite; Simultaneously the melt temperature of cristobalite in P-O system glass low relative to Si-O system glass 50 DEG C ~ 200 DEG C, accelerate the melting of quartz further, thus ceramic product can form excellent microstructure at a lower temperature: with acicular mullite and lime feldspar for principal crystalline phase, cristobalite is paracrystalline phase, and Si-O system and P-O system compound glass are Binder Phase.
(2) between the ceramic product principal crystalline phase that the present invention burns till after introducing tricalcium phosphate, between principal crystalline phase and glassy phase, thermal expansivity matches, and significantly can reduce the generation of tiny crack in sintering process, thus improves thermostability and the intensity of ceramic product.
Accompanying drawing explanation
Fig. 1 does not add the conventional ceramic Sample Scan electromicroscopic photograph (amplifying 5000 times) of tricalcium phosphate.
Fig. 2 embodiment 1 adds the stereoscan photograph (amplifying 5000 times) of the high tenacity ceramics sample of tricalcium phosphate.
Fig. 3 embodiment 1 adds the stereoscan photograph (amplifying 20000 times) of the high tenacity ceramics sample of tricalcium phosphate.
Fig. 4 does not add the X-ray diffraction analysis collection of illustrative plates of the conventional ceramic sample of tricalcium phosphate.
Fig. 5 embodiment 1 adds the X-ray diffraction analysis collection of illustrative plates of the high tenacity ceramics sample of tricalcium phosphate.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
Utilize tricalcium phosphate to prepare a method for high tenacity pottery, comprise the steps:
(1) by weight percentage, by tricalcium phosphate 15% and ceramic batch 85% (chemical group prejudice table 1) mixing, the mode mix grinding of ball milling evenly obtains slurry in a wet process; In wet ball grinding, the mass ratio of abrading-ball, mixture and water is: abrading-ball: mixture: water=1.2:1:0.8, and Ball-milling Time is 2h;
(2) slurry of step (1) is crossed 100 mesh sieves, in 100 DEG C of dry 24h, grind into powder, after 100 mesh sieves, dry-pressing formed, pressurize 1 minute obtained ceramic green under 15MPa;
(3) burnt till in kiln by ceramic green, controlling firing temperature is 1180 DEG C, and soaking time is 60 minutes, obtained ceramics sample;
Table 1 ceramic batch chemical constitution (wt%)
| Component | SiO 2 | Al 2O 3 | Fe 2O 3 | Na 2O | K 2O | CaO | P 2O 5 | MgO | Burn and lose |
| Blank | 70.27 | 18.01 | 0.48 | 0.80 | 1.90 | 0.45 | 0.23 | 0.25 | 7.61 |
Ceramic batch firing temperature in table 1 is 1270 DEG C, and detect by People's Republic of China (PRC) light industry standard QB/T1993-2012 (ceramic ware shock resistance experimental technique), product water-intake rate is 0.79%, resistance to impact shock is 1.95KJ/m
2; Do not introduce tricalcium phosphate, the conventional ceramic sample water-intake rate burnt till under 1180 DEG C of conditions by the ceramic batch in table 1 is 6.04%, and resistance to impact shock is 1.36KJ/m
2; After introducing 15% tricalcium phosphate, firing temperature 1180 DEG C, is incubated 60 minutes, the high tenacity ceramics sample burnt till after testing: water-intake rate is 0.47%, resistance to impact shock is 2.25KJ/m
2.
Burning till of pottery is the core procedure of production process, and its main purpose has two, and one is improve density, and two is improve intensity.The requirement that qualified product need density and intensity to reach certain.Described " the ceramic batch firing temperature in table 1 is 1270 DEG C ", refer to and ceramic batch is burnt till at 1270 DEG C, the performance requriements of product can be met, if lower than this temperature, the density (representing with water-intake rate) of stupalith and intensity (this sentences resistance to impact shock to represent) do not reach Standard.As 1180 DEG C of ceramic products burnt till, water-intake rate is higher, and illustrate that product porosity is comparatively large, density is inadequate; And resistance to impact shock is also lower than normal value.After introducing tricalcium phosphate, burn till at 1180 DEG C, ceramic product density and intensity, all higher than former blank 1270 DEG C of products burnt till, illustrate that preparation method, on the basis of enhancing product performance, can also reduce firing temperature, realize production energy-saving through improving.
In this embodiment, by introducing tricalcium phosphate, lime feldspar and Si-O system and P-O system compound glass phase can be generated in ceramic firing process.The introducing of calcareous element reduces the temperature that in sintering process, liquid phase occurs, changes the physico-chemical property of high-temperature liquid-phase, accelerates needle-like secondary mullite and is formed and quartzy melting; Simultaneously the melt temperature of quartz in P-O system glass low relative to Si-O system glass 50 DEG C ~ 200 DEG C, accelerate the melting of quartz further.Thus make ceramic product can form excellent microstructure at a lower temperature: with acicular mullite and lime feldspar for principal crystalline phase, cristobalite is paracrystalline phase, and Si-O system and P-O system compound glass are Binder Phase.
Do not add the scanning electron microscope collection of illustrative plates of the conventional ceramic sample of tricalcium phosphate as shown in Figure 1, principal crystalline phase is grainy texture; The present embodiment adds the scanning electron microscope collection of illustrative plates of the high tenacity ceramics sample of tricalcium phosphate as shown in Figures 2 and 3, and Fig. 2 is the collection of illustrative plates of amplification 5000 times, and Fig. 3 is the collection of illustrative plates of amplification 20000 times.Can find out from Fig. 2 and Fig. 3, principal crystalline phase is acicular structure.
Do not add the X-ray diffraction analysis collection of illustrative plates of the conventional ceramic sample of tricalcium phosphate as shown in Figure 4, product with cristobalite and mullite for principal crystalline phase; The present embodiment add tricalcium phosphate high tenacity ceramics sample X-ray diffraction analysis collection of illustrative plates as shown in Figure 5, product with lime feldspar, mullite for principal crystalline phase.
The present embodiment introduces the high tenacity ceramic product that burns till after tricalcium phosphate with lime feldspar and mullite for principal crystalline phase, matches, can reduce the generation of tiny crack in sintering process with Si-O system and P-O system compound glass thermal expansivity; And principal crystalline phase is acicular structure, therefore significantly can improve the resistance to impact shock of ceramic product, strengthen toughness of products.
The scanning electron microscope collection of illustrative plates of embodiment gained high tenacity ceramics sample is substantially identical with Fig. 2,3 below, and the X-ray diffraction analysis collection of illustrative plates of gained high tenacity ceramics sample is substantially identical with Fig. 5, provides no longer one by one.
Embodiment 2
Utilize tricalcium phosphate to prepare a method for high tenacity pottery, comprise the steps:
(1) by weight percentage, by tricalcium phosphate 10% and ceramic batch 90% (chemical group prejudice table 2) mixing, the mode mix grinding of ball milling evenly obtains slurry in a wet process; In wet ball grinding, the mass ratio of abrading-ball, mixture and water is: abrading-ball: mixture: water=1.2:1:0.8, and Ball-milling Time is 2h;
(2) slurry of step (1) is crossed 100 mesh sieves, in 100 DEG C of dry 24h, grind into powder, after 100 mesh sieves, dry-pressing formed, pressurize 1 minute obtained ceramic green under 15MPa;
(3) burnt till in kiln by ceramic green, controlling firing temperature is 1200 DEG C, and soaking time is 70 minutes, obtained ceramics sample;
Table 2 ceramic batch chemical constitution (wt%)
| Component | SiO 2 | Al 2O 3 | Fe 2O 3 | Na 2O | K 2O | CaO | P 2O 5 | MgO | Burn and lose |
| Blank | 68.34 | 19.41 | 0.44 | 0.83 | 1.81 | 0.15 | 0.10 | 0.48 | 8.44 |
Ceramic batch firing temperature in table 2 is 1290 DEG C, and detect by People's Republic of China (PRC) light industry standard QB/T1993-2012 (ceramic ware shock resistance experimental technique), product water-intake rate is 0.43%, resistance to impact shock is 2.05KJ/m
2; Do not introduce tricalcium phosphate, the conventional ceramic sample water-intake rate burnt till under 1200 DEG C of conditions by the ceramic batch in table 2 is 5.68%, and resistance to impact shock is 1.75KJ/m
2; After introducing 10% tricalcium phosphate, firing temperature 1200 DEG C, is incubated 70 minutes, the high tenacity ceramics sample burnt till after testing: water-intake rate is 0.27%, resistance to impact shock is 2.65KJ/m
2.
Embodiment 3
Utilize tricalcium phosphate to prepare a method for high tenacity pottery, comprise the steps:
(1) by weight percentage, by tricalcium phosphate 7% and ceramic batch 93% (chemical group prejudice table 3) mixing, the mode mix grinding of ball milling evenly obtains slurry in a wet process; In wet ball grinding, the mass ratio of abrading-ball, mixture and water is: abrading-ball: mixture: water=1.2:1:0.8, and Ball-milling Time is 2h;
(2) slurry of step (1) is crossed 100 mesh sieves, in 100 DEG C of dry 24h, grind into powder, after 100 mesh sieves, dry-pressing formed, pressurize 1 minute obtained ceramic green under 15MPa;
(3) burnt till in kiln by ceramic green, controlling firing temperature is 1240 DEG C, and soaking time is 80 minutes, obtained ceramics sample;
Table 3 ceramic batch chemical constitution (wt%)
| Component | SiO 2 | Al 2O 3 | Fe 2O 3 | Na 2O | K 2O | CaO | P 2O 5 | MgO | Burn and lose |
| Blank | 66.98 | 21.36 | 0.82 | 0.40 | 1.68 | 0.52 | 0.21 | 0.28 | 7.75 |
Ceramic batch firing temperature in table 3 is 1310 DEG C, and detect by People's Republic of China (PRC) light industry standard QB/T1993-2012 (ceramic ware shock resistance experimental technique), product water-intake rate is 0.38%, resistance to impact shock is 2.65KJ/m
2; Do not introduce tricalcium phosphate, the conventional ceramic sample water-intake rate burnt till under 1240 DEG C of conditions by the ceramic batch in table 3 is 6.04%, and resistance to impact shock is 2.16KJ/m
2; Introduce after tricalcium phosphate, firing temperature 1240 DEG C, is incubated 80 minutes, the high tenacity ceramics sample burnt till after testing: water-intake rate is 0.26%, resistance to impact shock is 2.95KJ/m
2.
Embodiment 4
Utilize tricalcium phosphate to prepare a method for high tenacity pottery, comprise the steps:
(1) by weight percentage, by tricalcium phosphate 5% and ceramic batch 95% (chemical group prejudice table 4) mixing, the mode mix grinding of ball milling evenly obtains slurry in a wet process; In wet ball grinding, the mass ratio of abrading-ball, mixture and water is: abrading-ball: mixture: water=1.2:1:0.8, and Ball-milling Time is 2h;
(2) slurry of step (1) is crossed 100 mesh sieves, in 100 DEG C of dry 24h, grind into powder, after 100 mesh sieves, dry-pressing formed, pressurize 1 minute obtained ceramic green under 15MPa;
(3) burnt till in kiln by ceramic green, controlling firing temperature is 1280 DEG C, and soaking time is 90 minutes, obtained ceramics sample;
Table 4 ceramic batch chemical constitution (wt%)
| Component | SiO 2 | Al 2O 3 | Fe 2O 3 | Na 2O | K 2O | CaO | P 2O 5 | MgO | Burn and lose |
| Blank | 65.14 | 22.56 | 0.37 | 0.97 | 2.24 | 0.28 | 0.11 | 0.13 | 8.20 |
Ceramic batch firing temperature in table 4 is 1320 DEG C, and detect by People's Republic of China (PRC) light industry standard QB/T1993-2012 (ceramic ware shock resistance experimental technique), product water-intake rate is 0.33%, shock resistance is 2.75KJ/m
2; Do not introduce tricalcium phosphate, the conventional ceramic sample water-intake rate burnt till under 1280 DEG C of conditions by the ceramic batch in table 4 is 1.04%, and resistance to impact shock is 2.35KJ/m
2; Introduce after tricalcium phosphate, firing temperature 1280 DEG C, is incubated 90 minutes, the high tenacity ceramics sample burnt till after testing: water-intake rate is 0.17%, resistance to impact shock is 3.05KJ/m
2.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. utilize tricalcium phosphate to prepare a method for high tenacity pottery, it is characterized in that comprising the steps:
(1) by tricalcium phosphate and ceramic batch mixing, the mode mix grinding of ball milling evenly obtains slurry in a wet process;
(2) step (1) gained slurry is sieved, dries, grind into powder, after sieve, dry-pressing formed, pressurize, obtained ceramic green;
(3) described ceramic green is burnt till in kiln, obtained high tenacity pottery;
The incorporation of step (1) described tricalcium phosphate accounts for 5% ~ 15% of tricalcium phosphate and ceramic batch total mass;
Composition and the mass percentage of step (1) described ceramic batch are: SiO
2: 65.14% ~ 70.27%, Al
2o
3: 18.01% ~ 22.56%, K
2o:1.68% ~ 2.24%, Na
2o:0.4% ~ 0.97%, MgO:0.13% ~ 0.48%, Fe
2o
3: 0.37% ~ 0.82%, CaO:0.15% ~ 0.52%, P
2o
5: 0.10% ~ 0.23%, burn mistake: 7.61% ~ 8.44%;
The temperature that step (3) described ceramic green burns till is 1180 ~ 1280 DEG C.
2. the method utilizing tricalcium phosphate to prepare high tenacity pottery according to claim 1, is characterized in that: the temperature of step (2) described oven dry is 100 DEG C.
3. the method utilizing tricalcium phosphate to prepare high tenacity pottery according to claim 1, is characterized in that: the pressure of step (2) described pressurize is 15MPa, and the dwell time is 1 minute.
4. the method utilizing tricalcium phosphate to prepare high tenacity pottery according to claim 1, is characterized in that: the temperature that step (3) described ceramic green burns till is 1200 ~ 1240 DEG C.
5. the method utilizing tricalcium phosphate to prepare high tenacity pottery according to claim 1, is characterized in that: the soaking time that step (3) described ceramic green burns till is 60 ~ 90 minutes.
6. the method utilizing tricalcium phosphate to prepare high tenacity pottery according to claim 5, is characterized in that: the soaking time that step (3) described ceramic green burns till is 70 ~ 80 minutes.
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| CN104860647A (en) * | 2015-04-13 | 2015-08-26 | 广东昌隆陶瓷股份有限公司 | Method for manufacturing high-strength egg-shell china |
| CN108329020A (en) * | 2018-03-05 | 2018-07-27 | 醴陵友立特种陶瓷有限公司 | The honeycomb ceramic heat accumulator and preparation method thereof of low adsorption ability |
| CN111233334B (en) * | 2020-02-25 | 2022-05-17 | 内蒙古工业大学 | Preparation method of anorthite-quartz-glass phase multiphase ceramic |
| CN111704441B (en) * | 2020-06-17 | 2022-03-25 | 蒙娜丽莎集团股份有限公司 | Blank body for high-strength thin ceramic plate, high-strength thin ceramic plate and preparation method of blank body |
| CN112299833B (en) * | 2020-09-30 | 2022-06-17 | 蒙娜丽莎集团股份有限公司 | High-strength high-toughness mullite ceramic sheet and preparation method thereof |
| CN115536361B (en) * | 2022-11-28 | 2023-05-02 | 蒙娜丽莎集团股份有限公司 | High-strength ceramic sheet and preparation method thereof |
| CN115991574B (en) * | 2023-03-24 | 2023-06-23 | 佛山市陶莹新型材料有限公司 | Wear-resistant corrosion-resistant ceramic glaze as well as preparation method and application thereof |
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| CN103396107A (en) * | 2013-07-19 | 2013-11-20 | 华南理工大学 | Method for preparing anorthite toughened ceramic by utilizing desulfurized gypsum |
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