CN115385672A - Opalescent porcelain powder and preparation method thereof - Google Patents

Opalescent porcelain powder and preparation method thereof Download PDF

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CN115385672A
CN115385672A CN202211144166.1A CN202211144166A CN115385672A CN 115385672 A CN115385672 A CN 115385672A CN 202211144166 A CN202211144166 A CN 202211144166A CN 115385672 A CN115385672 A CN 115385672A
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opalescent
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porcelain
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李蛟
鄢新章
刘谋山
郑杰
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Chengdu Besmile Biotechnology Co ltd
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Abstract

The invention relates to the technical field of ceramic materials, in particular to opalescent ceramic 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-scale leucite crystal, 79 to 89.9 percent of vitreous basic powder and 0.01 to 0.1 percent of inorganic pigment. The invention solves the problem that the milky white effect of the porcelain powder is uncontrollable in the prior art.

Description

Opalescent porcelain powder and preparation method thereof
Technical Field
The invention relates to the technical field of ceramic materials, in particular to opalescent ceramic powder and a preparation method thereof.
Background
The design idea of the opalescent effect porcelain is to mix colors according to different color requirements for use on the premise of meeting the performance of various porcelain powders. The imported opalescent porcelain powder has excellent aesthetic effect and physical and chemical properties, but is expensive; the opalescent porcelain powder produced by domestic manufacturers is relatively cheap, but the performance of the opalescent porcelain powder in terms of aesthetic effect and physical and chemical properties is inferior to that of the imported opalescent porcelain powder, and the opalescent porcelain powder is not widely accepted by the market.
At present, after the main types of porcelain powder such as common intrinsic porcelain, enamel porcelain and transparent porcelain are used, the porcelain powder is deficient 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 use of the opalescent effect porcelain can solve the problems that after the main types of porcelain powder such as the intrinsic porcelain, the enamel porcelain and the transparent porcelain are used, the aesthetic effect is poor, the translucency is not high and the like, so that the opalescent effect porcelain is more and more one of the main types of zirconia porcelain powder.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides opalescent porcelain powder and a preparation method thereof, which solve the problem that the opalescent effect of porcelain powder in the prior art is uncontrollable.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the invention discloses opalescent ceramic powder which comprises the following components in percentage by weight: 10.1 to 20 percent of micro-nano level 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 scale leucite crystals comprise, in weight percent: 45 to 65 percent of SiO 2 10 to 30 percent of Al 2 O 3 10% -30% of K 2 O, 1-10% of Na 2 O, 0.1-5% TiO 2 0.1 to 5 percent of Li 2 O, 0.1-5% SnO 2
Preferably, the vitreous base powder 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% of Na 2 O, caO 0.1-5%, baO 0.1-5%, tiO 0.1-5% 2 0.1 to 5 percent of ZrO 2 0.1 to 5 percent of Li 2 O、0.1%~5%SnO 2 2% -10% of B 2 O 3 0.1 to 5 percent of MgO and 0.01 to 2%F 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 coloring material 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: sintering the leucite crystal in a solid phase, and performing ball milling, drying and sieving to obtain the micro-nano leucite crystal; melting, opacifiing and grinding the vitreous basic powder and the inorganic pigment to obtain vitreous basic powder; mixing the micro-nano level leucite crystal and the vitreous basic powder, sintering, grinding, and spray drying to obtain the opalescent ceramic powder.
Preferably, the preparation process of the vitreous base powder comprises the following steps:
(1) Adding 8-24% of K 2 O, 1-10% of Na 2 O, baO 0.1-5 wt%, tiO 0.1-5 wt% 2 0.1 to 5 percent of ZrO 2 0.1 to 5 percent of Li 2 O、0.1%~5%SnO 2 2% -10% of B 2 O 3 0.1 to 5 percent of MgO and 0.01 to 2%P 2 O 5 0.01 to 1 percent of ZnO and 0.01 to 1 percent of Y 2 O 3 Mixing uniformly to obtain a mixture;
(2) 0.01 to 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 a rate of 4-10 ℃/min, preserving heat for 1-3 h, cooling, crushing, and mixing with 60-70% of SiO 2 Mixing to obtain adsorbent;
(4) Uniformly mixing the prepared adsorbent and the emulsion, standing for 1-3 h, adding the mixture, uniformly mixing, heating to 1500-1600 ℃ at a speed of 4-10 ℃/min, then preserving heat for 1-3 h, after the heat preservation is finished, preserving heat for 3-5 h at a temperature of 500-800 ℃ after the molten glass liquid is solidified, rapidly putting into cold water for water quenching, crushing, grinding and sieving by a 18-mesh sieve to obtain the vitreous base powder.
Preferably, the alumina comprises alpha alumina and gamma alumina, and the mass ratio of the alpha alumina to the gamma alumina 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, then the mixture is heated to 850-1100 ℃ at the speed of 5-8 ℃/min and is kept for 30-90 min, and after the heat preservation is finished, the mixture is put into water for cold quenching, and after being crushed, the mixture is sieved by a 18-mesh sieve, so that the opalescent effect porcelain base powder is obtained.
Preferably, the mass ratio of the opalescent effect porcelain base powder to the balls to the materials to the distilled water is (80-200): (10-100): (10-100) ball milling for 0.5-5 h, and spray drying to obtain the opalescent ceramic powder.
Preferably, the preparation process of the micro-nano scale leucite crystal comprises the following steps: uniformly mixing the leucite crystals, heating to 1200-1400 ℃ at the speed of 7-12 ℃/min, preserving heat for 1-3 h, cooling to room temperature, crushing, grinding and sieving with a 18-mesh sieve, wherein the mass ratio of balls, materials and distilled water is (80-200): (10-50): (10-50) ball milling for 1-24 h, drying, and sieving with a 200-mesh sieve to obtain the micro-nano leucite crystals.
The invention has the following beneficial effects:
according to the invention, alpha alumina and gamma alumina are added into vitreous base powder, calcium oxide is combined to prepare an adsorbent with micropores, silicon tetrafluoride is dissolved in ethanol and adsorbed by the adsorbent, and the adsorbent is combined with other components of the vitreous base powder to be sintered, so that the vitreous base powder is successfully prepared by adding the silicon tetrafluoride. The opalescent ceramic powder with controllable milky effect is prepared by combining phosphorus pentoxide and controlling the contents of silicon tetrafluoride and phosphorus pentoxide. Moreover, the sintered ceramic has the advantages of good natural opalescence effect, good permeability, high strength, high corrosion resistance and the like; in industrial preparation, the cost is lower, each preparation method is simple and easy to operate, and the commercialization of the opalescent porcelain powder can be effectively realized.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless otherwise indicated, the technical means used in the examples are conventional means well known to those skilled in the art.
In the invention, the proportion of the opalescent porcelain powder, the micro-nano-scale leucite crystal and the vitreous basic powder are calculated according to the mass percentage, so the percentage indicated in the proportion table disclosed by the invention is the percentage defined by the components in the respective formula. The percentage of manganese chloride as disclosed in table 4 was selected based on its formulation in the opalescent porcelain.
1. The invention discloses opalescent ceramic powder which comprises the following components in percentage by weight: 10.1 to 20 percent of micro-nano-scale leucite crystal, 79 to 89.9 percent of vitreous basic powder and 0.01 to 0.1 percent of inorganic pigment.
Wherein, according to the weight percentage, the micro-nano scale leucite crystal comprises: 45 to 65 percent of SiO 2 10 to 30 percent of Al 2 O 3 10% -30% of K 2 O, 1-10% of Na 2 O, 0.1-5% TiO 2 0.1 to 5 percent of Li 2 O, 0.1-5% SnO 2
The vitreous base powder includes: 60% -70% of SiO 2 10 to 20 percent of alumina and 8 to 24 percent of K 2 O, 1-10% of Na 2 O, caO 0.1-5%, baO 0.1-5%, tiO 0.1-5% 2 0.1 to 5 percent of ZrO 2 0.1 to 5 percent of Li 2 O、0.1%~5%SnO 2 2% -10% of B 2 O 3 0.1 to 5 percent of MgO and 0.01 to 2%F 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.
The invention adds phosphide and fluoride in the formula of the porcelain powder simultaneously, thus leading the glass to generate milky effect, if the fluoride is added independently, the opalescence effect of the fluoride on the glass is not strong, and the opalescence effect can be generated only by adding a large amount of fluoride, and when more fluoride is added, the strength of the finally produced porcelain powder can be influenced to a certain extent; and if the phosphide is added separately, the opacifying effect is too strong and is not easy to control, and when the glass added with the phosphide is poured out, the glass can be quickly opacified to generate the opalescence effect, so that the problem of nonuniform opacification of the glass (the inner part of the glass can be quickly opalescence) is generated. Therefore, the invention adjusts the proportion of fluoride and phosphide on the basis of the expected milky white effect, and enables the milky white effect to be more uniform in a controllable range.
2. The invention also discloses a preparation method of the opalescent ceramic powder, which comprises the following steps:
(1) Preparation of micro-nano scale leucite crystal
Weighing the components of the micro-nano scale leucite crystal according to the weight ratio of 1, uniformly mixing, heating to 1200-1400 ℃ at the speed of 7-12 ℃/min, preserving heat for 1-3 h, cooling to room temperature, crushing, grinding and sieving with a 18-mesh sieve, wherein the mass ratio of balls, materials and distilled water is (80-200): (10-50): (10-50) ball milling for 1-24 h, drying, and sieving with a 200-mesh sieve to obtain the micro-nano leucite crystals. The micro-nano scale leucite crystal prepared by the invention has controllable components and shape, has higher thermal expansion coefficient, and is generally (22-30) multiplied by 10 -6 The prepared porcelain powder has the advantages of continuously adjustable thermal expansion coefficient, the porcelain powder with different thermal expansion coefficients can be prepared according to specific needs in actual operation, and meanwhile, the white pomegranate crystals have refractive index close to that of the stone glass and cannot influence the required transparency of the porcelain powder due to strong diffuse scattering.
(2) Preparation of vitreous base powder
1) And 8 to 24 percent of K 2 O, 1-10% of Na 2 O, baO 0.1-5 wt%, tiO 0.1-5 wt% 2 0.1 to 5 percent of ZrO 2 0.1 to 5 percent of Li 2 O、0.1%~5%SnO 2 2% -10% of B 2 O 3 0.1 to 5 percent of MgO and 0.01 to 2%P 2 O 5 0.01 to 1 percent of ZnO and 0.01 to 1 percent of Y 2 O 3 Mixing evenly to obtain a mixture;
2) 0.01 to 2%F 4 Dissolving Si in 50-70% ethanol to obtain emulsion (namely silicon tetrafluoride ethanol solution) for later use; wherein, the mass fraction of the silicon tetrafluoride ethanol solution is 10-30%, and the dissolving 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, is adsorbed by the adsorbent and then is mixed with the mixture for high-temperature sintering, the opacifying effect is more uniform, and the problem of F is solved 4 Si is dispersed into the air to cause harm to human bodies. The ethanol may be in excess to completely dissolve F 4 Si is the standard.
3) Mixing 10-20% of alumina, 0.1-5% of CaO and inorganic pigment, heating to 1200-1600 ℃ at a rate of 4-10 ℃/min, preserving heat for 1-3 h, cooling, crushing, and mixing with 60-70% of SiO 2 Mixing to obtain adsorbent; 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 during high-temperature sintering, so that micropores with stable structures are obtained. The added gamma alumina can take two factors of material strength and stability into consideration, and the gamma alumina can generate crystal form change when the temperature is higher than 800 ℃, and simultaneously along with volume shrinkage, so that more open pores can be formed in the sintering process due to the crystal form transformation shrinkage of the gamma alumina, and the obtained open pores have smaller pore diameter, uniform distribution and good pore structure and are beneficial to absorbing emulsion due to smaller crystal nucleus of the gamma alumina.
4) Uniformly mixing the prepared adsorbent and the emulsion, and standing for 1-3 h; then adding the mixture to mix evenly, heating to 1500-1600 ℃ at 4-10 ℃/min, then preserving heat for 1-3 h, after the heat preservation is finished, after the molten glass liquid is solidified, preserving heat for 3-5 h at 500-800 ℃, then rapidly putting into cold water for water quenching, crushing and grinding, and sieving with a 18-mesh sieve to obtain the vitreous base powder. It should be noted that: during water quenching, the vitreous basic powder has milky white effect.
(3) Preparation of opalescent effect porcelain powder
Uniformly mixing the glass base powder and the micro-nano leucite crystals according to the mass ratio of 79-90 to 10-20, heating to 850-1100 ℃ at the speed of 5-8 ℃/min, preserving heat for 30-90 min, putting into water for cold quenching after heat preservation, crushing, and sieving with a 18-mesh sieve to obtain the opalescent-effect ceramic base powder. Mixing opalescent effect porcelain base powder with balls, materials and distilled water according to the mass ratio of (80-200): (10-100): (10-100) ball milling for 0.5-5 h, and spray drying to obtain the opalescent ceramic powder. The porcelain 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 porcelain powder matched with the thermal expansion coefficient of the zirconia full-porcelain ground crown can be prepared.
The invention is further illustrated by the following specific examples.
Examples
The preparation process was carried out according to method 2 above.
1. Preparation of micro-nano scale leucite crystal
Heating to 1350 ℃ at a heating rate of 10 ℃/min according to the mixture ratio shown in the following table 1, preserving heat for 2h, crushing, grinding and sieving with a 18-mesh sieve, ball-milling for 8h under the condition that the mass ratio of balls, materials and distilled water is 100.
TABLE 1 micro-nano level leucite Crystal composition (%)
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 mix ratios are shown in table 2 below. Before preparing the porcelain powder, the components were weighed according to the ratios in the following table.
TABLE 2 formulation of vitreous base powder (%)
Figure BDA0003854933130000071
3. Preparation of the emulsion
The formulation is shown in Table 3 below.
TABLE 3 formulation of emulsion (%)
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 the adsorbent
The formulation is shown in Table 4 below. Heating to 1400 deg.C at 8 deg.C/min, maintaining for 2 hr, cooling, pulverizing, mixing with SiO 2 Mixing to obtain the adsorbent. The control group was normal alumina.
TABLE 4 formulation of adsorbent (%)
Figure BDA0003854933130000072
Figure BDA0003854933130000081
5. Adsorption effect of adsorbent on emulsion
And (4) 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 silicon tetrafluoride ethanol solution in the remaining emulsion. The result shows that a plurality of micropores are formed after the alpha alumina, the gamma alumina and the calcium oxide are sintered at high temperature, so that the adsorption to the emulsion can be increased, and the content of silicon tetrafluoride in the preparation process of the opalescent ceramic powder can be controlled.
TABLE 5 adsorption effect of adsorbent
Figure BDA0003854933130000082
Figure BDA0003854933130000091
6. The adsorbents in table 5 which adsorb the emulsion were mixed with the mixture, and each group in table 5 was mixed with the corresponding group in table 2 to obtain 36 groups of vitreous base powders (for example, group a in table 2, based on alumina, α alumina and γ alumina were mixed with the other components in group a according to the three ratios in table 4, so that there were three groups of experiments in the ratio shown in group a, and the total of 36 groups of experiments in table 2). Heating to 1580 ℃ at the speed of 5 ℃/min, then preserving heat for 2h, after the heat preservation is finished, after the molten glass liquid is solidified, preserving heat for 4h at the temperature of 650 ℃, and then rapidly putting the glass liquid into cold water for water quenching, wherein the glass of each group has milky white effect and has different milky white degrees. Then crushing and grinding the water-quenched glass and sieving the crushed glass with a 18-mesh sieve to obtain vitreous base powder. In contrast, in comparative example 1, the cellophane base powder was obtained by directly mixing the components shown in Table 2 according to the above sintering parameters without preparing an emulsion. While comparative example 2 was the same as the preparation method of the present invention. The results show that the glass prepared in comparative example 1 has a problem of non-uniform opacification of the glass (the inside of the glass is rapidly milky white) when quenched with water. The glass prepared in comparative example 2 has a weak 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 scale leucite crystals according to a mass ratio of 89 to 10.95 (89 percent of the vitreous base powder, 10.95 percent of the micro-nano scale leucite crystals and 0.05 percent of inorganic pigment in percentage by mass), heating to 1000 ℃ at a speed of 5 ℃/min, preserving heat for 50min, after the heat preservation is finished, putting the mixture into water for cold quenching, crushing and then sieving with a 18-mesh sieve to obtain the opalescent effect ceramic base powder. Mixing opalescent effect porcelain base powder with balls, materials and distilled water according to the mass ratio of 100:30: ball milling is carried out for 3 hours under the condition of 30, and the opalescent effect porcelain powder is obtained after spray drying. The three-point bending strength and the thermal expansion coefficient are tested according to the method of GB 30367-2013 dental ceramic material. The results are shown in table 6 below, in which vitreous base powders prepared by selecting the compositions shown in group B6+ A3+ i were mixed with the compositions shown in table 1 to prepare opalescent porcelain powders, and the thermal expansion coefficient and three-point bending strength were measured.
Table 6 performance display of each group of porcelain powders
Figure BDA0003854933130000101
7.2 group B6+ A3+ i + group 2 in Table 6 was selected, opalescent effect porcelain powder was prepared according to the method of 7.1, chemical solubility test was performed according to the method in YY 0716-2009 "dental ceramics", and 10 samples and 6 samples were prepared for chemical solubility test and veneer porcelain strength test, respectively. The results are shown in Table 7 below.
TABLE 7 demonstration of the properties of the porcelain powders
Figure BDA0003854933130000111
8. The content and proportion of the silicon tetrafluoride and the phosphorus pentoxide have influence on the thermal expansion coefficient and the three-point bending strength of the porcelain powder. The micro-nano scale leucite crystals were prepared according to group 1 in table 1, and the adsorbent was prepared according to group B6 in table 5. The results are shown in Table 8 below.
TABLE 8 influence of the content and proportion of silicon tetrafluoride and phosphorus pentoxide on the porcelain powder properties
Figure BDA0003854933130000112
Figure BDA0003854933130000121
9. Adding mode for silicon tetrafluoride
(1) When the vitreous basic powder is sintered, the silicon tetrafluoride liquid is added after the vitreous basic powder is sintered, and as a result, the problem that the silicon tetrafluoride volatilizes because the silicon tetrafluoride is milky and very uneven only on the local part of the glass 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, a significant amount of silicon tetrafluoride gas is still present as a gas, while the water quenched glass has only a slight milky color on the surface and no or not much milky color inside.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.

Claims (10)

1. An opalescent porcelain powder is characterized in that: the paint comprises the following components in percentage by weight: 10.1 to 20 percent of micro-nano-scale leucite crystal, 79 to 89.9 percent of vitreous basic powder and 0.01 to 0.1 percent of inorganic pigment.
2. An opalescent porcelain powder according to claim 1, wherein: the micro-nano scale leucite crystal comprises the following components in percentage by weight: 45 to 65 percent of SiO 2 10 to 30 percent of Al 2 O 3 10% -30% of K 2 O, 1-10% of Na 2 O, 0.1-5% TiO 2 0.1 to 5 percent of Li 2 O, 0.1-5% SnO 2
3. An opalescent porcelain powder according to claim 1, characterized in that: the vitreous base powder 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% of Na 2 O, caO 0.1-5%, baO 0.1-5%, tiO 0.1-5% 2 0.1 to 5 percent of ZrO 2 0.1 to 5 percent of Li 2 O、0.1%~5%SnO 2 2% -10% of B 2 O 3 0.1 to 5 percent of MgO and 0.01 to 2%F 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
4. An opalescent porcelain powder according to claim 1, characterized in that: the inorganic pigment is at least one of erbium chloride, manganese chloride, praseodymium chloride and ferric chloride.
5. A preparation method of opalescent porcelain powder is characterized by comprising the following steps: the method comprises the following steps: sintering the leucite crystal in a solid phase, and performing ball milling, drying and sieving to obtain the micro-nano leucite crystal; melting, opacifiing and grinding the vitreous basic powder and the inorganic pigment to obtain vitreous basic powder; mixing the micro-nano level leucite crystal and the vitreous basic powder, sintering, grinding, and spray drying to obtain the opalescent ceramic powder.
6. The method for preparing the opalescent porcelain powder according to claim 5, wherein the method comprises the following steps: the preparation process of the vitreous basic powder comprises the following steps:
(1) Adding 8-24% of K 2 O, 1-10% of Na 2 O, baO 0.1-5 wt% and TiO 0.1-5 wt% 2 0.1 to 5 percent of ZrO 2 0.1 to 5 percent of Li 2 O、0.1%~5%SnO 2 2% -10% of B 2 O 3 0.1 to 5 percent of MgO and 0.01 to 2%P 2 O 5 0.01 to 1 percent of ZnO and 0.01 to 1 percent of Y 2 O 3 Mixing uniformly to obtain a mixture;
(2) 0.01 to 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 a rate of 4-10 ℃/min, preserving heat for 1-3 h, cooling, crushing, and mixing with 60-70% of SiO 2 Mixing to obtain adsorbent;
(4) Uniformly mixing the prepared adsorbent and the emulsion, standing for 1-3 h, adding the mixture, uniformly mixing, heating to 1500-1600 ℃ at a speed of 4-10 ℃/min, then preserving heat for 1-3 h, after the heat preservation is finished, preserving heat for 3-5 h at a temperature of 500-800 ℃ after the molten glass liquid is solidified, rapidly putting into cold water for water quenching, crushing, grinding and sieving by a 18-mesh sieve to obtain the vitreous base powder.
7. The method for preparing the opalescent porcelain powder according to claim 5, wherein the method comprises the following steps: the alumina comprises alpha alumina and gamma alumina, and the mass ratio of the alpha alumina to the gamma alumina is 8-9:1-2.
8. The method for preparing opalescent porcelain powder according to claim 5, wherein: uniformly mixing the vitreous basic powder and the micro-nano leucite crystals according to a mass ratio of 79-90.
9. The method for preparing the opalescent porcelain powder according to claim 8, wherein the method comprises the following steps: the mass ratio of the balls, the materials and the distilled water of the opalescent effect porcelain base powder is (80-200): (10-100): (10-100) ball milling for 0.5-5 h, and spray drying to obtain the opalescent ceramic powder.
10. The method for preparing the opalescent porcelain powder according to claim 5, wherein the method comprises the following steps: the preparation process of the micro-nano scale leucite crystal comprises the following steps: uniformly mixing the leucite crystals, heating to 1200-1400 ℃ at the speed of 7-12 ℃/min, preserving heat for 1-3 h, cooling to room temperature, crushing, grinding and sieving with a 18-mesh sieve, wherein the mass ratio of balls, materials and distilled water is (80-200): (10-50): (10-50) ball milling for 1-24 h, drying, and sieving with a 200-mesh sieve to obtain the micro-nano leucite crystals.
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DE603476C (en) * 1931-10-23 1934-10-03 Beryllium Dev Corp Separation of metals or metalloids forming water-soluble double fluorides from their compounds, in particular oxide or silicate ores containing foreign metals
CN101234851A (en) * 2008-03-04 2008-08-06 浙江大学 Method for preparing fluorine phosphorus composite opacifying glass
CN101244889A (en) * 2008-03-19 2008-08-20 山东轻工业学院 Non-fluorin environment protection opacifiedglass material and method for manufacturing same
CN109363952A (en) * 2018-11-29 2019-02-22 成都贝施美生物科技有限公司 A kind of porcelain powders and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE603476C (en) * 1931-10-23 1934-10-03 Beryllium Dev Corp Separation of metals or metalloids forming water-soluble double fluorides from their compounds, in particular oxide or silicate ores containing foreign metals
CN101234851A (en) * 2008-03-04 2008-08-06 浙江大学 Method for preparing fluorine phosphorus composite opacifying glass
CN101244889A (en) * 2008-03-19 2008-08-20 山东轻工业学院 Non-fluorin environment protection opacifiedglass material and method for manufacturing same
CN109363952A (en) * 2018-11-29 2019-02-22 成都贝施美生物科技有限公司 A kind of porcelain powders and preparation method thereof

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