CN109650724A - A kind of Lead-free transparent frit preparing ceramics - Google Patents
A kind of Lead-free transparent frit preparing ceramics Download PDFInfo
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- CN109650724A CN109650724A CN201910064537.7A CN201910064537A CN109650724A CN 109650724 A CN109650724 A CN 109650724A CN 201910064537 A CN201910064537 A CN 201910064537A CN 109650724 A CN109650724 A CN 109650724A
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- lead
- glaze
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Geochemistry & Mineralogy (AREA)
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Abstract
The invention discloses a kind of Lead-free transparent frits for preparing ceramics, and in particular to field of ceramic preparation, including major ingredient and auxiliary material, the major ingredient main chemical compositions include: SiO2、B2O2、Al2O3、ZnO、Li2O、Na2O、MgO、K2O and CaO, the auxiliary material main chemical compositions include: SrO, Bi2O3, Re, nitrate, titanium valve and vanadic anhydride.The present invention is fired by using lithium-containing compound or mineral spodumene and Suzhou soil as raw material, the chemical substance formed is fired to replace containing the PbO in lead glaze, it is formed together minimum eutectic, to substitute lead oxide, guarantee lower glaze firing temperature and wider firing range, both it can guarantee glaze glossiness, ensure that the coefficient of expansion matches, Li2O is the oxide with strong melting, can significantly reduce the coefficient of expansion of glaze and increase durability, add Li in frit2O can obtain gloss under lower temperature of glaze firing and elasticity is preferable, B2O2It can significantly reduce the melting temperature and viscosity of glaze, while can also act as strong fluxing agent.
Description
Technical field
The present invention relates to field of ceramic preparation technology, it is more particularly related to which a kind of prepare the unleaded of ceramics
Clear frit.
Background technique
Ceramic because it has the advantages that high compactness, good decorating effect, be widely used in daily necessities, construction material,
The fields such as the art work, but the frit of the general potting of the prior art is added with heavy metal lead more, the feature of environmental protection is poor, and general
Ceramic glaze be all it is opaque, brightness is poor, and color sense is bad, using lead as the ceramic glaze frit of primary raw material, have melting
The advantages that performance is excellent, and firing range is wide, but the lead contained containing lead frit has biggish toxicity to human body, and the prior art is general
That there are enamels is bad, opaque for the frit of potting, can cover to material color, cannot show the quality of material, and glaze light
The disadvantages of slippery is poor.It is therefore, a kind of Environmental Safety of R & D design, transparent it is necessary on the basis of the prior art,
Glossiness is good, is not easy loss of gloss, the Lead-free transparent frit of uniform color
The patent of invention of patent application publication CN201210191526.3 disclose it is a kind of prepare ceramics it is unleaded
Bright frit, it is made of the raw material of following parts by weight: SiO250~60 parts, Al2O310~20 parts, 1~5 part of MgO, CaO20
~30 parts, 10~20 parts of alkali metal salt.
But provided in above-mentioned technical proposal it is a kind of prepare ceramics Lead-free transparent frit practice constantly, still
It is old that there are more disadvantages to actually use if the material composition type in raw material is less being replaced into frit made of lead oxide
Preparation ceramics when, manufactured ceramic surface is more coarse, frit can bearing temperature it is lower, be easily damaged.
Summary of the invention
In order to overcome the drawbacks described above of the prior art, the embodiment of the present invention provides a kind of Lead-free transparent for preparing ceramics
Frit is fired as raw material by using lithium-containing compound or mineral spodumene and Suzhou soil, fires the chemicals of formation
Matter replaces containing the PbO in lead glaze, is formed together minimum eutectic, to substitute lead oxide, guarantees lower glaze firing temperature
With wider firing range, glaze glossiness both can guarantee, ensure that the coefficient of expansion matches, with K2O、Na2O is flux, can be made
Glaze has better glossiness, whiteness and transparency, but can significantly improve the glaze coefficient of expansion, Li again simultaneously2O is that have strong melt
Melt the oxide of effect, the coefficient of expansion of glaze can be significantly reduced and increase durability, contains Li in frit2O can be in lower glaze firing
At a temperature of obtain gloss and elasticity it is preferable, B2O2It can significantly reduce the melting temperature and viscosity of glaze, while can also act as strong fluxing
Agent.
To achieve the above object, the invention provides the following technical scheme: a kind of Lead-free transparent frit for preparing ceramics, packet
Major ingredient and auxiliary material are included, the major ingredient main chemical compositions include: SiO2、B2O2、Al2O3、 ZnO、Li2O、Na2O、MgO、K2O and
CaO, the auxiliary material main chemical compositions include: SrO, Bi2O3, Re, nitrate, titanium valve and vanadic anhydride, wherein major ingredient and
Each ingredient uses following proportion according to mass fraction in auxiliary material:: SiO28-16 parts, B2O24-8 parts, Al2O36-10 parts, ZnO 4-8
Part, Li26-8 parts of O, Na24-10 parts of O, 2-6 parts of MgO, K24-6 parts of O, 3-9 parts of CaO, 2-6 parts of SrO, Bi2O33 parts of 1-,
3-6 parts of Re, 1-2 parts of nitrate, 3-5 parts of titanium valve, 2-4 parts of vanadic anhydride.
In a preferred embodiment, the chemical component in the major ingredient chooses spodumene and Suzhou soil, the nitre
Hydrochlorate chooses sodium nitrate or potassium nitrate.
The present invention also provides a kind of preparation method of Lead-free transparent frit for preparing ceramics, specific steps are as follows:
Step 1: the titanium valve and vanadic anhydride chosen in auxiliary material are uniformly mixed, and ball milling then is added in the raw material of mixing
Ball-milling treatment is carried out in machine, is taken out and is dried for standby after the completion of processing；
Step 2: vacuum-sintering is carried out in the powder investment resistance furnace after drying in step 1, will be produced after the completion of sintering
It is spare that object is placed on cooling in cooling chamber；
Step 3: major ingredient is chosen, remaining auxiliary material is uniformly mixed with sintered product in step 2, and uniformly stirred
It mixes, stirring while is slowly added to nitrate；
Step 4: the raw material being configured in step 3 being added in smelting furnace and is heated, and mixing melt is heated to be clarification
Melt is taken out water quenching by the melt of homogenizing；
Step 5: carrying out drying and processing for the melt after water quenching, and pulverizer is added after drying and crushes, and will be smashed molten
For body by mesh screen, filtered product is frit.
In a preferred embodiment, the hot pressing pressure of resistance furnace is 10-15MPa in the step 2, and vacuum is burnt
Tie 2-4h.
In a preferred embodiment, in-furnace temperature being melted in the step 4,1200- is increased to 10-20 DEG C/min
1800 DEG C of firings, fire 6-8h.
Technical effect and advantage of the invention:
1, the present invention is fired by using lithium-containing compound or mineral spodumene and Suzhou soil as raw material, fires shape
At chemical substance replace containing the PbO in lead glaze, be formed together minimum eutectic, to substitute lead oxide, guarantee lower glaze
Face firing temperature and wider firing range both can guarantee glaze glossiness, ensure that the coefficient of expansion matches, with K2O、Na2O
It for flux, can make glaze that there is better glossiness, whiteness and transparency, but the glaze coefficient of expansion can be significantly improved again simultaneously,
Li2O is the oxide with strong melting, can significantly reduce the coefficient of expansion of glaze and increase durability, contain Li in frit2O
Gloss can be obtained under lower temperature of glaze firing and elasticity is preferable, while the glaze that the coefficient of expansion is small, B2O2It can significantly reduce the melting of glaze
Temperature and viscosity, while can also act as strong fluxing agent；
2, agent is made improvements using rare earth element, the formation of frit glass network can be remarkably promoted in the glaze that induces one on a small quantity, improved
The moist and brightness of glaze can achieve the purpose for improving glaze quality, while contain Al in raw material2O3, can limited drop
The melting temperature of low glaze improves the glossiness of glaze；
3, by will mix after titanium valve and vanadic anhydride processing with major ingredient, titanium valve and vanadic anhydride are burnt by vacuum
Knot, increases titanium aluminium inter-layer bonding force, to greatly improve the intensity and hardness of material, it is whole can to enhance manufactured frit
Stability.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment one:
The present invention provides a kind of Lead-free transparent frit for preparing ceramics, including major ingredient and auxiliary material, the major ingredient are main
Chemical component includes: SiO2、B2O2、Al2O3、ZnO、Li2O、Na2O、MgO、K2O and CaO, the auxiliary material main chemical compositions packet
It includes: SrO, Bi2O3, Re, nitrate, titanium valve and vanadic anhydride, wherein each ingredient is used according to mass fraction in major ingredient and auxiliary material
It matches below: SiO28 parts, B2O24 parts, Al2O36 parts, 4 parts of ZnO, Li26 parts of O, Na24 parts of O, 2 parts of MgO, K24 parts of O, CaO
3 parts, 2 parts of SrO, Bi2O31 part, 3 parts of Re, 1 part of nitrate, 3 parts of titanium valve, 2 parts of vanadic anhydride.
Chemical component in the major ingredient chooses spodumene and Suzhou soil, and the nitrate chooses sodium nitrate or potassium nitrate.
The present invention also provides a kind of preparation method of Lead-free transparent frit for preparing ceramics, specific steps are as follows:
Step 1: the titanium valve and vanadic anhydride chosen in auxiliary material are uniformly mixed, and ball milling then is added in the raw material of mixing
Ball-milling treatment is carried out in machine, is taken out and is dried for standby after the completion of processing；
Step 2: vacuum-sintering is carried out in the powder investment resistance furnace after drying in step 1, will be produced after the completion of sintering
Object is placed in cooling chamber that cooling is spare, and the hot pressing pressure of resistance furnace is 10MPa, vacuum-sintering 4h；
Step 3: major ingredient is chosen, remaining auxiliary material is uniformly mixed with sintered product in step 2, and uniformly stirred
It mixes, stirring while is slowly added to nitrate；
Step 4: the raw material being configured in step 3 being added in smelting furnace and is heated, and mixing melt is heated to be clarification
Melt is taken out water quenching by the melt of homogenizing, and molten in-furnace temperature increases to 1800 DEG C of firings with 10 DEG C/min, fires 6h；
Step 5: carrying out drying and processing for the melt after water quenching, and pulverizer is added after drying and crushes, and will be smashed molten
For body by mesh screen, filtered product is frit.
Embodiment two:
The present invention provides a kind of Lead-free transparent frit for preparing ceramics, including major ingredient and auxiliary material, the major ingredient are main
Chemical component includes: SiO2、B2O2、Al2O3、ZnO、Li2O、Na2O、MgO、K2O and CaO, the auxiliary material main chemical compositions packet
It includes: SrO, Bi2O3, Re, nitrate, titanium valve and vanadic anhydride, wherein each ingredient is used according to mass fraction in major ingredient and auxiliary material
It matches below:: SiO216 parts, B2O28 parts, Al2O310 parts, 8 parts of ZnO, Li28 parts of O, Na210 parts of O, 6 parts of MgO, K2O 6
Part, 9 parts of CaO, 6 parts of SrO, Bi2O33 parts, 6 parts of Re, 2 parts of nitrate, 5 parts of titanium valve, 4 parts of vanadic anhydride.
Chemical component in the major ingredient chooses spodumene and Suzhou soil, and the nitrate chooses sodium nitrate or potassium nitrate.
The present invention also provides a kind of preparation method of Lead-free transparent frit for preparing ceramics, specific steps are as follows:
Step 1: the titanium valve and vanadic anhydride chosen in auxiliary material are uniformly mixed, and ball milling then is added in the raw material of mixing
Ball-milling treatment is carried out in machine, is taken out and is dried for standby after the completion of processing；
Step 2: vacuum-sintering is carried out in the powder investment resistance furnace after drying in step 1, will be produced after the completion of sintering
Object is placed in cooling chamber that cooling is spare, and the hot pressing pressure of resistance furnace is 15MPa, vacuum-sintering 2h；
Step 3: major ingredient is chosen, remaining auxiliary material is uniformly mixed with sintered product in step 2, and uniformly stirred
It mixes, stirring while is slowly added to nitrate；
Step 4: the raw material being configured in step 3 being added in smelting furnace and is heated, and mixing melt is heated to be clarification
Melt is taken out water quenching by the melt of homogenizing, and molten in-furnace temperature increases to 1200 DEG C of firings with 20 DEG C/min, fires 6h；
Step 5: carrying out drying and processing for the melt after water quenching, and pulverizer is added after drying and crushes, and will be smashed molten
For body by mesh screen, filtered product is frit.
Embodiment three:
The present invention provides a kind of Lead-free transparent frit for preparing ceramics, including major ingredient and auxiliary material, the major ingredient are main
Chemical component includes: SiO2、B2O2、Al2O3、ZnO、Li2O、Na2O、MgO、K2O and CaO, the auxiliary material main chemical compositions packet
It includes: SrO, Bi2O3, Re, nitrate, titanium valve and vanadic anhydride, wherein each ingredient is used according to mass fraction in major ingredient and auxiliary material
It matches below:: SiO212 parts, B2O26 parts, Al2O38 parts, 6 parts of ZnO, Li27 parts of O, Na27 parts of O, 4 parts of MgO, K25 parts of O,
6 parts of CaO, 4 parts of SrO, Bi2O32 parts, 4 parts of Re, 1.5 parts of nitrate, 4 parts of titanium valve, 3 parts of vanadic anhydride.
Chemical component in the major ingredient chooses spodumene and Suzhou soil, and the nitrate chooses sodium nitrate or potassium nitrate.
The present invention also provides a kind of preparation method of Lead-free transparent frit for preparing ceramics, specific steps are as follows:
Step 1: the titanium valve and vanadic anhydride chosen in auxiliary material are uniformly mixed, and ball milling then is added in the raw material of mixing
Ball-milling treatment is carried out in machine, is taken out and is dried for standby after the completion of processing；
Step 2: vacuum-sintering is carried out in the powder investment resistance furnace after drying in step 1, will be produced after the completion of sintering
Object is placed in cooling chamber that cooling is spare, and the hot pressing pressure of resistance furnace is 13MPa, vacuum-sintering 3h；
Step 3: major ingredient is chosen, remaining auxiliary material is uniformly mixed with sintered product in step 2, and uniformly stirred
It mixes, stirring while is slowly added to nitrate；
Step 4: the raw material being configured in step 3 being added in smelting furnace and is heated, and mixing melt is heated to be clarification
Melt is taken out water quenching by the melt of homogenizing, and molten in-furnace temperature increases to 1500 DEG C of firings with 15 DEG C/min, fires 7h；
Step 5: carrying out drying and processing for the melt after water quenching, and pulverizer is added after drying and crushes, and will be smashed molten
For body by mesh screen, filtered product is frit.
Example IV:
By potassium feldspar, albite, quartz, lime stone, dolomite, spodumene, lepidolite and Suzhou soil phase when selection major ingredient
Same weight is fired test, and chemical substance contained by the substance for firing generation is recorded, specific content of chemical substances
Data are as follows:
It is obtained after test, the required content of chemical substances that spodumene and Suzhou soil contain in sintering procedure is most complete
Face, while loss on ignition is few, can be improved production efficiency.
Agent is made improvements using rare earth element in ingredient simultaneously, the shape of frit glass network can be remarkably promoted in the glaze that induces one on a small quantity
At, improve the moist and brightness of glaze, can achieve improve glaze quality purpose.
Last: the foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, all in the present invention
Spirit and principle within, any modification, equivalent replacement, improvement and so on, should be included in protection scope of the present invention it
It is interior.
Claims (4)
1. a kind of Lead-free transparent frit for preparing ceramics, including major ingredient and auxiliary material, it is characterised in that: the major ingredient primary chemical
Ingredient includes: SiO2、B2O2、Al2O3、ZnO、Li2O、Na2O、MgO、K2O and CaO, the auxiliary material main chemical compositions include:
SrO、Bi2O3, Re, nitrate, titanium valve and vanadic anhydride, wherein in major ingredient and auxiliary material each ingredient according to mass fraction use with
Lower proportion:: 8-16 parts of SiO2, B2O24-8 parts, Al2O36-10 parts, 4-8 parts of ZnO, Li26-8 parts of O, Na24-10 parts of O,
2-6 parts of MgO, K24-6 parts of O, 3-9 parts of CaO, 2-6 parts of SrO, Bi2O31-3 parts, 3-6 parts of Re, 1-2 parts of nitrate, titanium valve
3-5 parts, 2-4 parts of vanadic anhydride.
2. a kind of Lead-free transparent frit for preparing ceramics according to claim 1, it is characterised in that: in the major ingredient
Chemical component chooses spodumene and Suzhou soil, and the nitrate chooses sodium nitrate or potassium nitrate.
3. a kind of preparation method for the Lead-free transparent frit for preparing ceramics described in -2 any one according to claim 1,
It is characterized in that: specific steps are as follows:
Step 1: the titanium valve and vanadic anhydride chosen in auxiliary material are uniformly mixed, and then the raw material of mixing is added in ball mill
Ball-milling treatment is carried out, takes out and is dried for standby after the completion of processing；
Step 2: vacuum-sintering is carried out in the powder investment resistance furnace after drying in step 1, puts product after the completion of sintering
It is spare to set the cooling in cooling chamber；
Step 3: selection major ingredient, remaining auxiliary material are uniformly mixed with sintered product in step 2, and carry out uniform stirring, are stirred
Nitrate is slowly added to while mixing；
Step 4: the raw material being configured in step 3 being added in smelting furnace and is heated, and mixing melt is heated to be clarifying and homogenizing
Melt, melt is taken out into water quenching；
Step 5: carrying out drying and processing for the melt after water quenching, and pulverizer is added after drying and crushes, and smashed melt is led to
Mesh screen is crossed, filtered product is frit.
4. a kind of preparation method of Lead-free transparent frit for preparing ceramics according to claim 3, it is characterised in that: institute
The hot pressing pressure for stating resistance furnace in step 2 is 10-15MPa, vacuum-sintering 2-4h.It is according to claim 3 a kind of to prepare
The preparation method of the Lead-free transparent frit of ceramics, it is characterised in that: in-furnace temperature is melted in the step 4 with 10-20 DEG C/min
1200-1800 DEG C of firing is increased to, 6-8h is fired.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627359A (en) * | 2019-11-04 | 2019-12-31 | 江西飞宇新能源科技有限公司 | Frit for glaze and preparation method thereof |
| CN117303741A (en) * | 2023-10-19 | 2023-12-29 | 潮州市潮安区唯高品厨卫有限公司 | High-temperature-resistant glaze |
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| CN110627359A (en) * | 2019-11-04 | 2019-12-31 | 江西飞宇新能源科技有限公司 | Frit for glaze and preparation method thereof |
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| CN117303741B (en) * | 2023-10-19 | 2024-03-08 | 潮州市潮安区唯高品厨卫有限公司 | High-temperature-resistant glaze |
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Application publication date: 20190419 |