CN115385672B - Opalescent porcelain powder and preparation method thereof - Google Patents
Opalescent porcelain powder and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 104
- 229910052573 porcelain Inorganic materials 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000000694 effects Effects 0.000 claims abstract description 42
- 239000013078 crystal Substances 0.000 claims abstract description 40
- 229910052907 leucite Inorganic materials 0.000 claims abstract description 34
- 239000001023 inorganic pigment Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims description 34
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 27
- 239000000839 emulsion Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000003463 adsorbent Substances 0.000 claims description 17
- 238000007873 sieving Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 11
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 10
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 10
- 238000010791 quenching Methods 0.000 claims description 9
- 230000000171 quenching effect Effects 0.000 claims description 9
- 229910018068 Li 2 O Inorganic materials 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 6
- 238000001694 spray drying Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000006060 molten glass Substances 0.000 claims description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 4
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 4
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 4
- 235000002867 manganese chloride Nutrition 0.000 claims description 4
- 239000011565 manganese chloride Substances 0.000 claims description 4
- 229940099607 manganese chloride Drugs 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- HDGGAKOVUDZYES-UHFFFAOYSA-K erbium(iii) chloride Chemical compound Cl[Er](Cl)Cl HDGGAKOVUDZYES-UHFFFAOYSA-K 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- LHBNLZDGIPPZLL-UHFFFAOYSA-K praseodymium(iii) chloride Chemical compound Cl[Pr](Cl)Cl LHBNLZDGIPPZLL-UHFFFAOYSA-K 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims description 2
- 239000000049 pigment Substances 0.000 claims 7
- 239000002994 raw material Substances 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 4
- 239000011521 glass Substances 0.000 description 16
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 12
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 8
- 239000000292 calcium oxide Substances 0.000 description 7
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 235000013365 dairy product Nutrition 0.000 description 4
- 230000010494 opalescence Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- YSBQKZZHQPPKEL-UHFFFAOYSA-N ethanol;tetrafluorosilane Chemical compound CCO.F[Si](F)(F)F YSBQKZZHQPPKEL-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000011351 dental ceramic Substances 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000002223 garnet Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 241000219991 Lythraceae Species 0.000 description 1
- 235000014360 Punica granatum Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- ULGYAEQHFNJYML-UHFFFAOYSA-N [AlH3].[Ca] Chemical compound [AlH3].[Ca] ULGYAEQHFNJYML-UHFFFAOYSA-N 0.000 description 1
- 239000011805 ball Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000005337 ground glass Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011022 opal Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C03—GLASS; MINERAL OR SLAG WOOL
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Abstract
The invention relates to the technical field of ceramic materials, in particular to opalescent porcelain powder and a preparation method thereof. The specific technical scheme is as follows: the opalescent porcelain powder comprises the following components in percentage by weight: 10.1 to 20 percent of micro-nano leucite crystal, 79 to 89.9 percent of vitreous base powder and 0.01 to 0.1 percent of inorganic pigment. The invention solves the problem that the milky effect of the porcelain powder is uncontrollable in the prior art.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to opalescent porcelain powder and a preparation method thereof.
Background
The design idea of opalescent effect porcelain is to carry out color mixing according to different color requirements on the premise of meeting the performances of various porcelain powders. The imported emulsion porcelain powder has excellent aesthetic effect and physical and chemical properties, but has high price; the price of the dairy porcelain powder produced by domestic manufacturers is relatively low, but the performance of the dairy porcelain powder is inferior to that of imported dairy porcelain powder in aesthetic effect and physical and chemical properties, and the dairy porcelain powder has not been widely accepted by the market.
The prior common porcelain powder with main types such as intrinsic porcelain, enamel porcelain, transparent porcelain and the like has defects in gloss and translucency compared with natural teeth, the natural teeth have good milky gloss and high translucency at cut ends and adjacent parts of the teeth, and the opalescent effect porcelain can supplement the problems of poor aesthetic effect, low translucency and the like of the porcelain powder with main types such as the intrinsic porcelain, the enamel porcelain, the transparent porcelain and the like after being used, so that the opalescent effect porcelain becomes one of the main types of zirconia porcelain powder more and more.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides opalescent porcelain powder and a preparation method thereof, and solves the problem that the opalescent effect of porcelain powder in the prior art is uncontrollable.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the invention discloses opalescent porcelain powder which comprises the following components in percentage by weight: 10.1 to 20 percent of micro-nano leucite crystal, 79 to 89.9 percent of vitreous base powder and 0.01 to 0.1 percent of inorganic pigment.
Preferably, the micro-nano garnet crystal comprises, in weight percent: 45% -65% of SiO 2 10 to 30 percent of Al 2 O 3 10-30% of K 2 O, 1-10% Na 2 O, 0.1-5% TiO 2 0.1 to 5 percent of Li 2 0.1 to 5 percent of O and 0.1 to 5 percent of SnO 2 。
Preferably, the vitreous base powder comprises, in weight percent: 60% -70% of SiO 2 10 to 20 percent of alumina and 8 to 24 percent of K 2 O, 1-10% Na 2 O, 0.1 to 5 percent of CaO, 0.1 to 5 percent of BaO and 0.1 to 5 percent of TiO 2 ZrO 0.1% -5% 2 0.1 to 5 percent of Li 2 O、0.1％～5％SnO 2 2-10% of B 2 O 3 MgO in 0.1-5 wt% and MgO in 0.01-2%F wt% 4 Si、0.01％～2％P 2 O 5 0.01 to 1 percent of ZnO and 0.01 to 1 percent of Y 2 O 3 。
Preferably, the inorganic pigment is at least one of erbium chloride, manganese chloride, praseodymium chloride and ferric chloride.
Correspondingly, the preparation method of the opalescent porcelain powder comprises the following steps: solid-phase sintering the leucite crystal, and then ball milling, drying and sieving the leucite crystal to obtain the micro-nano leucite crystal; melting, opacifying and grinding the vitreous base powder and the inorganic pigment to obtain the vitreous base powder; mixing the micro-nano leucite crystals and the vitreous base powder, and then sintering, grinding and spray drying to obtain the opalescent effect porcelain powder.
Preferably, the preparation process of the vitreous base powder comprises the following steps:
(1) 8 to 24 percent of K 2 O, 1-10% Na 2 O, 0.1 to 5 percent of BaO and 0.1 to 5 percent of TiO 2 ZrO 0.1% -5% 2 0.1 to 5 percent of Li 2 O、0.1％～5％SnO 2 2-10% of B 2 O 3 MgO in 0.1-5 wt% and MgO in 0.01-2%P wt% 2 O 5 0.01 to 1 percent of ZnO and 0.01 to 1 percent of Y 2 O 3 Uniformly mixing to obtain a mixture;
(2) Will be 0.01% -2%F 4 Dissolving Si in 50-70% ethanol to obtain emulsion for later use;
(3) Mixing 10-20% of alumina, 0.1-5% of CaO and inorganic pigment, heating to 1200-1600 ℃ at 4-10 ℃/min, preserving heat for 1-3 h, cooling, pulverizing, mixing with 60-70% of SiO 2 Mixing to obtain adsorbent for use;
(4) Uniformly mixing the prepared adsorbent and emulsion, standing for 1-3 h, adding the mixture, uniformly mixing, heating to 1500-1600 ℃ at 4-10 ℃/min, preserving heat for 1-3 h, preserving heat, solidifying molten glass after the heat preservation is finished, preserving heat for 3-5 h at 500-800 ℃, rapidly placing into cold water for water quenching, crushing, grinding and sieving with a 18-mesh sieve to obtain the vitreous base powder.
Preferably, the alumina comprises alpha alumina and gamma alumina, and the mass ratio is 8-9:1-2.
Preferably, the vitreous base powder and the micro-nano leucite crystal are uniformly mixed according to the mass ratio of 79-90:10-20, then the temperature is raised to 850-1100 ℃ at 5-8 ℃/min, the heat is preserved for 30-90 min, after the heat preservation is finished, the mixture is put into water for cold quenching, crushed and then screened by a 18-mesh sieve, and the opalescent effect porcelain base powder is obtained.
Preferably, the opalescent effect porcelain base powder comprises the following components in parts by mass: (10-100): ball milling is carried out for 0.5 to 5 hours under the condition of (10 to 100), and the opalescent effect porcelain powder is obtained by spray drying.
Preferably, the preparation process of the micro-nano leucite crystal comprises the following steps: uniformly mixing leucite crystals, heating to 1200-1400 ℃ at a speed of 7-12 ℃/min, preserving heat for 1-3 h, cooling to room temperature, crushing, grinding, sieving with a 18-mesh sieve, and mixing the materials with distilled water according to the mass ratio of (80-200): (10-50): ball milling for 1-24 h under the condition of (10-50), drying, and sieving with a 200-mesh sieve to obtain the micro-nano leucite crystal.
The invention has the following beneficial effects:
according to the invention, alpha alumina and gamma alumina are added into the vitreous base powder, calcium oxide is combined to prepare the adsorbent with micropores, silicon tetrafluoride is dissolved in ethanol and is adsorbed by the adsorbent, and other components of the vitreous base powder are combined to sinter, so that silicon tetrafluoride is successfully added to prepare the vitreous base powder. And the opalescent porcelain powder with controllable opalescence effect is prepared by combining phosphorus pentoxide and controlling the contents of silicon tetrafluoride and phosphorus pentoxide. Moreover, the ceramic material has the advantages of good natural opalescence effect, good permeability, high strength, high corrosion resistance and the like after sintering; in industrial preparation, the cost is lower, and each preparation method is simple and easy to operate, so that commercialization of the opalescent porcelain powder can be effectively realized.
Detailed Description
The following description will clearly and fully describe the technical solutions of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The technical means used in the examples are conventional means well known to those skilled in the art unless otherwise indicated.
In the invention, the proportion of opal porcelain powder, micro-nano leucite crystal and vitreous base powder are calculated according to mass percent, so the percentages in the proportion table disclosed by the invention are defined according to the percentages of the components in the respective formulas. The percentage of manganese chloride as disclosed in table 4 was selected based on its proportion in opalescent porcelain powder.
1. The invention discloses opalescent porcelain powder which comprises the following components in percentage by weight: 10.1 to 20 percent of micro-nano leucite crystal, 79 to 89.9 percent of vitreous base powder and 0.01 to 0.1 percent of inorganic pigment.
Wherein, according to weight percent, the micro-nano leucite crystal comprises: 45% -65% of SiO 2 10 to 30 percent of Al 2 O 3 10-30% of K 2 O, 1-10% Na 2 O、0.1 to 5 percent of TiO 2 0.1 to 5 percent of Li 2 0.1 to 5 percent of O and 0.1 to 5 percent of SnO 2 。
The vitreous base powder comprises: 60% -70% of SiO 2 10 to 20 percent of alumina and 8 to 24 percent of K 2 O, 1-10% Na 2 O, 0.1 to 5 percent of CaO, 0.1 to 5 percent of BaO and 0.1 to 5 percent of TiO 2 ZrO 0.1% -5% 2 0.1 to 5 percent of Li 2 O、0.1％～5％SnO 2 2-10% of B 2 O 3 MgO in 0.1-5 wt% and MgO in 0.01-2%F wt% 4 Si、0.01％～2％P 2 O 5 0.01 to 1 percent of ZnO and 0.01 to 1 percent of Y 2 O 3 。
The inorganic pigment is at least one of erbium chloride, manganese chloride, praseodymium chloride and ferric chloride.
According to the invention, phosphide and fluoride are added into the formula of the porcelain powder at the same time, so that the glass has a milky effect, if fluoride is added singly, the opacifying effect of fluoride on the glass is not strong, and a large amount of fluoride is added to generate the opacifying effect, and when more fluoride is added, the strength of the finally produced porcelain powder is influenced to a certain extent; the emulsion effect is too strong and is not easy to control when phosphide is added alone, and the emulsion effect can be quickly formed by emulsion after the phosphide is poured out, so that the problem of uneven emulsion of the glass (the inside of the glass can be quickly milky) is generated. Therefore, the invention can make the milky effect more uniform in a controllable range on the basis of the expected milky effect by adjusting the proportion of the fluoride and the phosphide on the basis.
2. The invention also discloses a preparation method of the opalescent porcelain powder, which comprises the following steps:
(1) Preparation of micro-nano leucite crystal
Weighing the components of the micro-nano leucite crystal according to the formula 1, uniformly mixing, heating to 1200-1400 ℃ at 7-12 ℃/min, preserving heat for 1-3 h, cooling to room temperature, crushing, grinding, sieving with a 18-mesh sieve, and mixing with the following components in percentage by mass (80-200): (10-50): ball milling is carried out for 1 to 24 hours under the condition of (10 to 50),drying and sieving with a 200-mesh sieve to obtain micro-nano leucite crystals. The micro-nano leucite crystal prepared by the invention has controllable components and shape, higher thermal expansion coefficient, and is generally (22-30) multiplied by 10 -6 And (K) the ceramic powder prepared by the method has the advantages of continuously adjustable thermal expansion coefficients, ceramic powder with different thermal expansion coefficients can be prepared according to specific requirements in actual operation, and meanwhile, the white garnet crystal also has the refractive index close to that of stone glass, so that the transparency required by the ceramic powder is not influenced by strong diffuse scattering.
(2) Preparation of vitreous base powder
1) 8 to 24 percent of K 2 O, 1-10% Na 2 O, 0.1 to 5 percent of BaO and 0.1 to 5 percent of TiO 2 ZrO 0.1% -5% 2 0.1 to 5 percent of Li 2 O、0.1％～5％SnO 2 2-10% of B 2 O 3 MgO in 0.1-5 wt% and MgO in 0.01-2%P wt% 2 O 5 0.01 to 1 percent of ZnO and 0.01 to 1 percent of Y 2 O 3 Uniformly mixing to obtain a mixture;
2) Will be 0.01 to 2%F 4 Dissolving Si in 50-70% ethanol to obtain emulsion (i.e. silicon tetrafluoride ethanol solution) for later use; wherein the mass fraction of the silicon tetrafluoride ethanol solution is 10-30%, and the dissolution time is 1-4 h. Due to F 4 Si is gas and can not be directly added into the material, so that the Si is dissolved in ethanol, and is mixed with the mixture for high-temperature sintering after being adsorbed by the adsorbent, so that not only is the opacifying effect more uniform, but also F is solved 4 Si is scattered into the air to cause harm to human body. The ethanol may be in excess to completely dissolve F 4 Si is the right.
3) Mixing 10-20% of alumina, 0.1-5% of CaO and inorganic pigment, heating to 1200-1600 ℃ at 4-10 ℃/min, preserving heat for 1-3 h, cooling, pulverizing, mixing with 60-70% of SiO 2 Mixing to obtain adsorbent for use; wherein the alumina comprises alpha alumina and gamma alumina, and the mass ratio is 8-9:1-2. It should be noted that: calcium oxide and alpha alumina form calcium aluminum crystal form in high temperature sintering, so as to obtain stable structureIs a micro-pore of (a). The added gamma alumina can take account of two factors of material strength and stability, and when the gamma alumina is higher than 800 ℃, crystal form change occurs, and simultaneously volume shrinkage is accompanied, so that in the sintering process, more open pores can be formed due to crystal form transformation shrinkage of the gamma alumina, and the obtained open pores have smaller pore diameters, uniform distribution and good pore structure, thereby being beneficial to adsorbing emulsion.
4) Uniformly mixing the prepared adsorbent and emulsion, and standing for 1-3 h; then adding the mixture, uniformly mixing, heating to 1500-1600 ℃ at 4-10 ℃/min, preserving heat for 1-3 h, after the heat preservation is finished, solidifying the molten glass, preserving heat for 3-5 h at 500-800 ℃, rapidly putting into cold water for water quenching, crushing, grinding and sieving with a 18-mesh sieve to obtain the vitreous base powder. It should be noted that: upon water quenching, the vitreous base powder exhibits a milky effect.
(3) Preparation of opalescent effect porcelain powder
Uniformly mixing vitreous base powder and micro-nano leucite crystals according to the mass ratio of 79-90:10-20, heating to 850-1100 ℃ at 5-8 ℃/min, preserving heat for 30-90 min, putting into water for cold quenching after the heat preservation is finished, and sieving with a 18-mesh sieve after crushing to obtain opalescent effect porcelain base powder. The opalescent effect porcelain base powder comprises the following components in percentage by mass (80-200): (10-100): ball milling is carried out for 0.5 to 5 hours under the condition of (10 to 100), and the opalescent effect porcelain powder is obtained by spray drying. The ceramic powder prepared by mixing the white pomegranate crystals and the vitreous base powder has the characteristic of continuously adjustable thermal expansion coefficient, and meanwhile, the opalescent ceramic powder matched with the thermal expansion coefficient of the zirconia full ceramic bottom crown can be prepared.
The invention is further illustrated below in conjunction with specific examples.
Examples
The preparation process was carried out according to method 2 described above.
1. Preparation of micro-nano leucite crystal
According to the proportion shown in the following table 1, the temperature is raised to 1350 ℃ at a heating rate of 10 ℃/min, then the mixture is kept for 2 hours, crushed, ground and screened by a 18-mesh sieve, ball milling is carried out for 8 hours under the condition that the mass ratio of balls, materials and distilled water is 100:30:30, and the mixture is dried and screened by a 200-mesh sieve, thus obtaining the micro-nano leucite crystal.
TABLE 1 proportion of micro-nano-sized leucite crystals (%)
| Group of | SiO 2 | Al 2 O 3 | K 2 O | Na 2 O | TiO 2 | Li 2 O | SnO 2 |
| Group 1 | 45 | 29 | 13 | 6 | 2.5 | 2.5 | 2 |
| Group 2 | 49 | 25 | 13 | 6 | 2.5 | 2.5 | 2 |
| Group 3 | 59 | 15 | 13 | 6 | 2.5 | 2.5 | 2 |
| Group 4 | 64 | 10 | 13 | 6 | 2.5 | 2.5 | 2 |
2. Preparation of vitreous base powder
The proportions of the mixtures are shown in Table 2 below. Before preparing the porcelain powder, the components were weighed according to the proportions shown in the following table.
TABLE 2 formulation of vitreous base powder (%)
3. Preparation of the emulsion
The proportions are shown in Table 3 below.
TABLE 3 emulsion formulation (%)
| Group of | F 4 Si | Mass fraction of ethanol | Mass fraction of silicon tetrafluoride ethanol solution |
| Group A1 | 0.01 | 65 | 10 |
| Group A2 | 0.5 | 65 | 10 |
| Group A3 | 1 | 65 | 20 |
| Group A4 | 2 | 65 | 30 |
4. Preparation of adsorbents
The proportions are shown in Table 4 below. Heating to 1400 ℃ at 8 ℃/min, preserving heat for 2h, cooling, pulverizing, mixing with SiO 2 Mixing to obtain the adsorbent. The control group is common alumina.
Table 4 proportion of adsorbents (%)
5. Adsorption effect of adsorbent on emulsion
And (3) uniformly mixing the adsorbent and the emulsion, and standing for 2 hours. The results are shown in Table 5 below. As a result, the adsorption effect was evaluated by the content of the siliconoxide tetrafluoride solution in the remaining emulsion. The result shows that after the alpha alumina, the gamma alumina and the calcium oxide are sintered at high temperature, a plurality of micropores are formed, and the adsorption of emulsion can be increased, so that the content of silicon tetrafluoride in the preparation process of the emulsion porcelain powder is controlled.
TABLE 5 adsorption Effect of adsorbents
6. The adsorbents of the adsorption emulsion of table 5 were mixed with the mixture, and each group of table 5 was mixed in accordance with table 2 to obtain 36 groups of vitreous base powders (for example, group a of table 2, based on alumina, alpha alumina and gamma alumina were mixed with the other components of group a in three proportions of table 4, so that there were three experiments for the proportions shown in group a, and the total of 36 experiments for the whole table 2). After the temperature is raised to 1580 ℃ at 5 ℃ per minute, the glass is kept for 2 hours, after the molten glass is solidified after the temperature is kept, the molten glass is quickly put into cold water for water quenching after the temperature is kept for 4 hours at 650 ℃, at this time, the effect of milky white is achieved on all groups of glass, and the milky white degree is different. And then crushing and grinding the water quenched glass, and sieving the crushed and ground glass with a 18-mesh sieve to obtain the vitreous base powder. In contrast, in comparative example 1, the glass paper base powder was obtained directly according to the above sintering parameters in accordance with the proportions shown in Table 2 without preparing an emulsion. Comparative example 2 is the same as the preparation method of the present invention. The results show that the glass prepared in comparative example 1, when quenched with water, had a problem of uneven glass opacification (rapid milky white inside the glass). The glass prepared in comparative example 2 had a poor opacifying effect on the glass when quenched with water.
7. Preparation of opalescent effect porcelain powder
7.1, uniformly mixing the vitreous base powder and the micro-nano leucite crystal according to the mass ratio of 89:10.95 (89% of the vitreous base powder, 10.95% of the micro-nano leucite crystal and 0.05% of the inorganic pigment according to the mass percentage), heating to 1000 ℃ at 5 ℃/min, preserving heat for 50min, putting into water for quenching after the heat preservation is finished, and sieving with a 18-mesh sieve after crushing to obtain the opalescent effect porcelain base powder. The opalescent effect porcelain base powder is prepared from the following components in percentage by mass: 30: ball milling is carried out for 3 hours under the condition of 30, and the opalescent effect porcelain powder is obtained by spray drying. The test of the three-point flexural strength and the thermal expansion coefficient was carried out according to the method of GB 30367-2013 "dental ceramic Material". The results are shown in Table 6 below, wherein the vitreous base powders prepared in the proportions shown in the groups B6+A3+i were selected, and the respective proportions shown in Table 1 were mixed to prepare the emulsion porcelain powders, and the thermal expansion coefficients and the three-point flexural strength were measured.
Table 6 Performance display of porcelain powders of each group
7.2 selecting group B6+A3+i+group 2 of Table 6, preparing opalescent effect porcelain powder according to the method of 7.1, performing chemical solubility test according to the method in YY 0716-2009 "dental ceramics", and preparing 10 samples and 6 samples respectively for chemical solubility test and facing porcelain strength test. The results are shown in Table 7 below.
Table 7 Performance display of porcelain powders
8. Influence of the content and proportion of silicon tetrafluoride and phosphorus pentoxide on the thermal expansion coefficient and three-point bending strength of the porcelain powder. The proportion of micro-nano-sized leucite crystals was as set 1 in table 1 and the adsorbents were prepared as set B6 in table 5. The results are shown in Table 8 below.
TABLE 8 influence of the contents and proportions of silicon tetrafluoride and phosphorus pentoxide on the properties of porcelain powders
9. Mode of addition for silicon tetrafluoride
(1) The silicon tetrafluoride is directly pressed and condensed into liquid, and when the vitreous base powder is sintered, the silicon tetrafluoride liquid is added after the sintering of the vitreous base powder is completed, and as a result, the problem that the silicon tetrafluoride volatilizes due to the fact that milky white color only appears on part of glass and is very uneven is found.
(2) In the process of sintering the vitreous base powder, sintering is performed in an atmosphere containing silicon tetrafluoride gas. The results show that after sintering is completed, a large amount of silicon tetrafluoride gas is still present as a gas, while the water quenched glass has only a slight opalescence on the surface and no or too much opalescence inside.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (8)
1. A preparation method of opalescent porcelain powder is characterized in that: the method comprises the following steps: solid-phase sintering the leucite crystal, and then ball milling, drying and sieving the leucite crystal to obtain the micro-nano leucite crystal; melting, opacifying and grinding the vitreous base powder and the inorganic pigment to obtain pigment-containing vitreous base powder; mixing micro-nano leucite crystals and vitreous base powder containing pigment, and then sintering, grinding and spray drying to obtain opalescent effect ceramic powder;
the preparation process of the vitreous base powder containing pigment comprises the following steps:
(1) 8 to 24 percent of K 2 O, 1-10% Na 2 O, 0.1 to 5 percent of BaO and 0.1 to 5 percent of TiO 2 ZrO 0.1% -5% 2 0.1 to 5 percent of Li 2 O、0.1%～5%SnO 2 2-10% of B 2 O 3 MgO in 0.1-5 wt% and MgO in 0.01-2%P wt% 2 O 5 0.01 to 1 percent of ZnO and 0.01 to 1 percent of Y 2 O 3 Uniformly mixing to obtain a mixture;
(2) Will be 0.01% -2%F 4 Dissolving Si in 50-70% ethanol to obtain emulsion for later use;
(3) Mixing 10-20% of alumina, 0.1-5% of CaO and inorganic pigment, heating to 1200-1600 ℃ at 4-10 ℃/min, preserving heat for 1-3 h, cooling, pulverizing, mixing with 60-70% of SiO 2 Mixing to obtain adsorbent for use;
(4) Uniformly mixing the prepared adsorbent and emulsion, standing for 1-3 h, adding the mixture, uniformly mixing, heating to 1500-1600 ℃ at 4-10 ℃/min, preserving heat for 1-3 h, preserving heat, solidifying molten glass after the heat preservation is finished, preserving heat for 3-5 h at 500-800 ℃, rapidly placing into cold water for water quenching, crushing, grinding and sieving with a 18-mesh sieve to obtain vitreous base powder containing pigment;
wherein, the opalescent effect porcelain powder comprises the following raw materials in percentage by weight: 10.1 to 20 percent of micro-nano leucite crystal, 79 to 89.9 percent of vitreous basic powder containing pigment and 0.01 to 0.1 percent of inorganic pigment;
the vitreous base powder containing pigment comprises the following components in percentage by weight: 60% -70% of SiO 2 10 to 20 percent of alumina and 8 to 24 percent of K 2 O, 1-10% Na 2 O, 0.1 to 5 percent of CaO, 0.1 to 5 percent of BaO and 0.1 to 5 percent of TiO 2 ZrO 0.1% -5% 2 、0.1%～5% Li 2 O、0.1%～5%SnO 2 2-10% of B 2 O 3 MgO in 0.1-5 wt% and MgO in 0.01-2%F wt% 4 Si、0.01%～2%P 2 O 5 0.01 to 1 percent of ZnO and 0.01 to 1 percent of Y 2 O 3 。
2. The method for preparing opalescent porcelain powder according to claim 1, which is characterized in that: the alumina comprises alpha alumina and gamma alumina, and the mass ratio is 8-9:1-2.
3. The method for preparing opalescent porcelain powder according to claim 1, which is characterized in that: uniformly mixing the vitreous base powder containing the pigment and the micro-nano leucite crystal, heating to 850-1100 ℃ at 5-8 ℃/min, preserving heat for 30-90 min, putting into water for cold quenching after preserving heat, crushing, and sieving with a 18-mesh sieve to obtain the opalescent effect porcelain base powder.
4. A method for preparing opalescent porcelain powder according to claim 3, which is characterized in that: the opalescent effect porcelain base powder comprises the following components in parts by mass: (10-100): ball milling is carried out for 0.5 to 5 hours under the condition of (10 to 100), and the opalescent effect porcelain powder is obtained by spray drying.
5. The method for preparing opalescent porcelain powder according to claim 1, which is characterized in that: the preparation process of the micro-nano leucite crystal comprises the following steps: uniformly mixing leucite crystal raw materials, heating to 1200-1400 ℃ at a speed of 7-12 ℃/min, preserving heat for 1-3 h, cooling to room temperature, crushing, grinding, sieving with a 18-mesh sieve, and mixing the materials with distilled water according to the mass ratio of (80-200): (10-50): ball milling for 1-24 h under the condition of (10-50), drying, and sieving with a 200-mesh sieve to obtain the micro-nano leucite crystal.
6. An opalescent porcelain powder produced by the production method of claim 1.
7. According to the weightsA opalescent porcelain powder as defined in claim 6 wherein: the micro-nano leucite crystal comprises the following components in percentage by weight: 45% -65% of SiO 2 10 to 30 percent of Al 2 O 3 10-30% of K 2 O, 1-10% Na 2 O, 0.1-5% TiO 2 0.1 to 5 percent of Li 2 0.1 to 5 percent of O and 0.1 to 5 percent of SnO 2 。
8. The opalescent porcelain powder of claim 6 wherein: the inorganic pigment is at least one of erbium chloride, manganese chloride, praseodymium chloride and ferric chloride.
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