CN113372113A - Preparation method of polycrystalline zirconium gem - Google Patents
Preparation method of polycrystalline zirconium gem Download PDFInfo
- Publication number
- CN113372113A CN113372113A CN202110750546.9A CN202110750546A CN113372113A CN 113372113 A CN113372113 A CN 113372113A CN 202110750546 A CN202110750546 A CN 202110750546A CN 113372113 A CN113372113 A CN 113372113A
- Authority
- CN
- China
- Prior art keywords
- zirconium
- solution
- mixed solution
- minutes
- polycrystalline
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The embodiment of the disclosure discloses a preparation method of a polycrystalline zirconium gem. One embodiment of the method comprises: adding zirconium oxychloride into purified water to completely dissolve the zirconium oxychloride to obtain a zirconium oxychloride solution; generating zirconium sulfate solid based on zirconium oxychloride solution and sodium sulfate; dissolving the zirconium sulfate solid in purified water, and adding yttrium chloride and magnesium chloride solution for mixing to obtain a mixed solution; adding an alkali solution to the mixed solution to completely separate out a solid precipitate; drying and pre-sintering the solid precipitate; introducing purified water, a colorant, a water-soluble organic dispersant, a water-soluble polymer stabilizer and a pre-sintered substance into a ball mill filled with alumina grinding balls to carry out homogenization grinding treatment to obtain a mixed suspension; and carrying out spray drying treatment on the mixed suspension to obtain the polycrystalline zirconium gem material. This embodiment increases the hardness of the zirconium gemstones produced.
Description
Technical Field
The embodiment of the disclosure relates to the field of zirconium gem preparation, in particular to a polycrystalline zirconium gem preparation method.
Background
Currently, zirconia is widely used in the fields of refractory materials, grinding tools, solid fuel cells, jewelry and the like. The preparation of zirconia is generally carried out in the following manner: cold crucible method.
However, with the above-described preparation, there are generally the following technical problems:
first, the hardness of zirconia (zircon stone) prepared by the cold crucible method is low;
second, the color of the zirconia prepared by the cold crucible method is single.
Disclosure of Invention
This summary is provided to introduce a selection of concepts in a simplified form that are further described below in the detailed description. This summary is not intended to identify key features or essential features of the claimed subject matter, nor is it intended to be used to limit the scope of the claimed subject matter.
Some embodiments of the present disclosure propose polycrystalline zirconium gemstone preparation methods to solve one or more of the technical problems mentioned in the background section above.
Some embodiments of the present disclosure provide a method of preparing a polycrystalline zirconium gemstone, the method comprising: adding zirconium oxychloride into purified water to completely dissolve the zirconium oxychloride to obtain a zirconium oxychloride solution; generating a zirconium sulfate solid based on the zirconium oxychloride solution and sodium sulfate, wherein the mass of the sodium sulfate is 1-2 times of that of the zirconium oxychloride; dissolving the zirconium sulfate solid in purified water, and adding yttrium chloride and magnesium chloride solution for mixing to obtain a mixed solution; adding an alkali solution to the mixed solution to completely separate out a solid precipitate; drying and pre-sintering the solid precipitate; introducing purified water, a colorant, a water-soluble organic dispersant, a water-soluble polymer stabilizer and a pre-sintered substance into a ball mill filled with alumina grinding balls to carry out homogenization grinding treatment to obtain a mixed suspension; and carrying out spray drying treatment on the mixed suspension to obtain the polycrystalline zirconium gem material.
The above embodiments of the present disclosure have the following advantages: by the polycrystalline zirconium gemstone preparation method of some embodiments of the present disclosure, the hardness of the prepared zirconium gemstone is improved. Based on this, in the polycrystalline zirconia gemstone preparation method of some embodiments of the present disclosure, first, zirconium oxychloride is added to purified water to be completely dissolved, resulting in a zirconium oxychloride solution. Therefore, the subsequent reaction with sodium sulfate is convenient to produce zirconium sulfate solid. Next, a zirconium sulfate solid was produced based on the above zirconium oxychloride solution and sodium sulfate. And then, putting the zirconium sulfate solid into purified water for dissolving, and adding yttrium chloride and magnesium chloride solution for mixing to obtain a mixed solution. Wherein the mixed solution comprises zirconium oxide, magnesium oxide and yttrium oxide. Thus, a solution containing zirconium oxide can be obtained, and subsequent zirconium gem generation is facilitated. Next, an alkali solution was added to the above mixed solution to completely precipitate a solid precipitate. Then, the solid precipitate is dried and presintered. Thereby, the solid precipitate can be sintered into solid particles. Then, purified water, a colorant, a water-soluble organic dispersant, a water-soluble polymer stabilizer and a pre-sintered substance are introduced into a ball mill equipped with alumina grinding balls to perform a homogenizing grinding treatment, resulting in a mixed suspension. Thus, the surface tension of the solid particles is removed by the water-soluble organic dispersant, and the solid particles are uniformly dispersed in the solution. The water-soluble polymer stabilizer is used for improving the hardness of the prepared zirconium gem. In addition, the homogenization grinding treatment is performed by a ball mill, so that the colorant, the water-soluble organic dispersant, the water-soluble polymer stabilizer and the pre-sintered substance can be sufficiently and uniformly mixed. Here, the polycrystalline zirconium gem material prepared subsequently can be made to present various colors by using the coloring agent. And finally, carrying out spray drying treatment on the mixed suspension to obtain the polycrystalline zirconium gem material. Therefore, the hardness of the prepared zirconium gem is improved.
Drawings
The above and other features, advantages and aspects of various embodiments of the present disclosure will become more apparent by referring to the following detailed description when taken in conjunction with the accompanying drawings. Throughout the drawings, the same or similar reference numbers refer to the same or similar elements. It should be understood that the drawings are schematic and that elements and elements are not necessarily drawn to scale.
FIG. 1 is a flow chart of some embodiments of a method of making a polycrystalline zirconium gemstone according to the present disclosure;
FIG. 2 is a flow chart of still further embodiments of methods of making polycrystalline zirconium gemstones according to the present disclosure.
Detailed Description
Embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While certain embodiments of the present disclosure are shown in the drawings, it is to be understood that the disclosure may be embodied in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided for a more thorough and complete understanding of the present disclosure. It should be understood that the drawings and embodiments of the disclosure are for illustration purposes only and are not intended to limit the scope of the disclosure.
It should be noted that, for convenience of description, only the portions related to the related invention are shown in the drawings. The embodiments and features of the embodiments in the present disclosure may be combined with each other without conflict.
It should be noted that the terms "first", "second", and the like in the present disclosure are only used for distinguishing different devices, modules or units, and are not used for limiting the order or interdependence relationship of the functions performed by the devices, modules or units.
It is noted that references to "a", "an", and "the" modifications in this disclosure are intended to be illustrative rather than limiting, and that those skilled in the art will recognize that "one or more" may be used unless the context clearly dictates otherwise.
The names of messages or information exchanged between devices in the embodiments of the present disclosure are for illustrative purposes only, and are not intended to limit the scope of the messages or information.
The present disclosure will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
Fig. 1 is a flow chart 100 of some embodiments of methods of making polycrystalline zirconium gemstones according to some embodiments of the present disclosure. The method may be performed by a process robot. The preparation method of the polycrystalline zirconium gem comprises the following steps:
In some embodiments, the main body of the polycrystalline zirconia gemstone preparation method (process machine equipment, where the process machine equipment may include equipment such as a process robot, a heating device (furnace), a cooling device, a spray dryer, etc.) may take a preset mass of zirconium oxychloride and add the zirconium oxychloride to pure water having a mass 3 to 5 times that of the zirconium oxychloride to perform complete dissolution, resulting in a zirconium oxychloride solution. Here, the setting of the preset quality is not limited. For example, the preset mass may be 10 kilograms.
In some embodiments, the performing body may generate zirconium sulfate solids based on the zirconium oxychloride solution and sodium sulfate. Wherein the mass of the sodium sulfate is 1-2 times of that of the zirconium oxychloride.
In practice, based on the zirconium oxychloride solution and sodium sulfate described above, a zirconium sulfate solid can be produced by:
firstly, adding the sodium sulfate into the zirconium oxychloride solution to obtain a zirconium sulfate mixed solution. Here, the sodium sulfate may be added to the zirconium oxychloride solution and sufficiently stirred to obtain a zirconium sulfate mixed solution. Here, the sodium sulfate may be up to anhydrous sodium sulfate
Secondly, heating the zirconium sulfate mixed solution to 74-76 ℃, and then cooling the zirconium sulfate mixed solution at 74-76 ℃ to 29-31 ℃. Here, the heating rate of heating may be 5 ℃/min. The cooling may be to rest.
And thirdly, filtering the zirconium sulfate mixed solution cooled to 29-31 ℃ to obtain zirconium sulfate solid. The filtration method is not limited here.
103, putting the zirconium sulfate solid in purified water for dissolving, and adding yttrium chloride and magnesium chloride solution for mixing to obtain a mixed solution.
In some embodiments, the execution body may dissolve the zirconium sulfate solid in purified water having a mass ten times that of the zirconium sulfate solid, and add yttrium chloride and magnesium chloride solutions to mix, thereby obtaining a mixed solution. Here, the mass ratio of the yttrium chloride and magnesium chloride solution to the zirconium sulfate solid may be: (0.5-3): 100. here, the mixed solution may include zirconia, yttria, magnesia, and the like.
In some embodiments, the performing body may add the alkali solution to the mixed solution to completely precipitate the solid precipitate by:
firstly, controlling the temperature range of the mixed solution to be 30-50 ℃, and continuously dripping an alkali solution into the mixed solution and stirring for 20 minutes to obtain a first stirred mixed solution. Wherein the pH value of the alkali solution is more than 7 and less than 9, and the stirring speed is 100 r/min. Here, the amount of the alkali solution per drop is 0.04ml to 0.05 ml.
And secondly, controlling the temperature range of the first stirring mixed solution to be 55-75 ℃, and continuously dripping a first alkali solution into the first stirring mixed solution and stirring for 10 minutes to obtain a second stirring mixed solution. Wherein the pH value of the first alkali solution is more than or equal to 9 and less than 10, and the stirring speed is 150 revolutions per minute. Here, the amount of the first alkali solution per drop is 0.04ml to 0.05 ml.
And thirdly, controlling the temperature of the second stirring mixed solution to be 74-76 ℃, and continuously dripping a second alkali solution into the second stirring mixed solution and stirring for 5 minutes to obtain a third stirring mixed solution. Wherein the pH value of the second alkali solution is more than or equal to 10 and less than 13, and the stirring speed is 100 revolutions per minute. Here, the second alkali solution is 0.04ml to 0.05ml per drop.
And fourthly, controlling the temperature of the third stirring mixed solution to be 74-76 ℃, and stirring for 30 minutes to completely separate out solid precipitates. Wherein the stirring speed is 10 r/min.
And 105, drying and pre-sintering the solid precipitate.
In some embodiments, the performing body may perform the drying and pre-sintering process on the solid precipitate by:
firstly, carrying out spray drying treatment on the solid precipitate to obtain a dry solid precipitate. Here, the solid precipitate may be subjected to a spray drying treatment by a spray dryer.
And a second step of performing the following presintering step on the dried solid precipitate:
in a first substep, the above dried solid precipitate is heated to 300 ℃ and held for 30 minutes in response to heating to 300 ℃. Wherein the heating rate is 5 ℃/min. In practice, the execution body may heat the dried solid precipitate to 300 ℃ by a heating device, and incubate for 30 minutes in response to heating the dried solid precipitate to 300 ℃.
A second substep of heating the dried solid precipitate at 300 ℃ after 30 minutes of incubation to 1300 ℃ and incubating for 60 minutes in response to heating to 1300 ℃. Wherein the heating rate is 10 ℃/min. In practice, the above-described execution main body may heat the dried solid precipitate having a temperature of 300 ℃ after the incubation for 30 minutes to 1300 ℃ by the heating means, and incubate for 60 minutes in response to heating the dried solid precipitate having a temperature of 300 ℃ after the incubation for 30 minutes to 1300 ℃.
A third substep of cooling the dried solid precipitate at 1300 ℃ after 60 minutes of incubation to 1100 ℃ and incubating for 10 minutes in response to cooling to 1100 ℃. Wherein the cooling rate is 10 ℃/min. In practice, the above-described execution main body may cool the dried solid precipitate having a temperature of 1300 ℃ after the incubation for 60 minutes to 1100 ℃ by the cooling device, and incubate for 10 minutes in response to cooling the dried solid precipitate having a temperature of 1300 ℃ after the incubation for 60 minutes to 1100 ℃.
And a fourth substep of cooling the dried solid precipitate at the temperature of 1100 ℃ after heat preservation for 10 minutes to 800 ℃, and standing and cooling to 24-26 ℃ in response to the cooling to 800 ℃, wherein the cooling rate of the cooling is 20 ℃/minute. In practice, the execution main body can cool the dried solid precipitate with the temperature of 1100 ℃ after the heat preservation for 10 minutes to 800 ℃ at the cooling rate of 20 ℃/minute, and response to the cooling to 800 ℃, stand and cool to 24-26 ℃.
And 106, introducing purified water, the coloring agent, the water-soluble organic dispersant, the water-soluble polymer stabilizer and the pre-sintered substance into a ball mill filled with alumina grinding balls to perform homogenization grinding treatment to obtain a mixed suspension.
In some embodiments, the above-described execution body may introduce purified water, a colorant, a water-soluble organic dispersant, a water-soluble polymer stabilizer, and a pre-sintered substance into a ball mill equipped with alumina milling balls to perform a homogenizing milling process, resulting in a mixed suspension. Here, the mass of the purified water is 8 to 10 times of that of the pre-sintered material. Here, the pre-sintered material includes zirconia. The pre-sintered mass may also include yttria and magnesia. The water-soluble organic dispersant includes, but is not limited to, one or more of the following: ammonium citrate polyacrylate and polyethyleneimine. The mass ratio of the water-soluble organic dispersant to the zirconia is as follows: (0.01-1.5): 100. here, the grinding method of the above-mentioned homogenization grinding treatment is ball milling. Wherein, the ball milling speed is as follows: 60-200 r/min, wherein the ball milling time is as follows: 120-180 minutes. Here, the colorant may include, but is not limited to, one or more of the following: ferroferric oxide, cobaltous oxide, aluminum oxide and terbium heptaoxide.
And 107, carrying out spray drying treatment on the mixed suspension to obtain the polycrystalline zirconium gem material.
In some embodiments, the performing body may perform a spray drying process on the mixed suspension to obtain a polycrystalline zirconium gem material. Here, the polycrystalline zirconia stone material may refer to polycrystalline zirconia stone powder. Here, the grain size of the grains of the polycrystalline zircon stone powder is 1 μm or less. Here, the polycrystalline zirconium gem powder may include, but is not limited to, by mass percent: zirconia (70-94%), oxide stabilizer (3-5%), colorant (2-25%), etc. Here, the oxide stabilizer may include yttrium oxide and magnesium oxide.
The above embodiments of the present disclosure have the following advantages: by the polycrystalline zirconium gemstone preparation method of some embodiments of the present disclosure, the hardness of the prepared zirconium gemstone is improved. Based on this, in the polycrystalline zirconia gemstone preparation method of some embodiments of the present disclosure, first, zirconium oxychloride is added to purified water to be completely dissolved, resulting in a zirconium oxychloride solution. Therefore, the subsequent reaction with sodium sulfate is convenient to produce zirconium sulfate solid. Next, a zirconium sulfate solid was produced based on the above zirconium oxychloride solution and sodium sulfate. And then, putting the zirconium sulfate solid into purified water for dissolving, and adding yttrium chloride and magnesium chloride solution for mixing to obtain a mixed solution. Wherein the mixed solution comprises zirconium oxide, magnesium oxide and yttrium oxide. Thus, a solution containing zirconium oxide can be obtained, and subsequent zirconium gem generation is facilitated. Next, an alkali solution was added to the above mixed solution to completely precipitate a solid precipitate. Then, the solid precipitate is dried and presintered. Thereby, the solid precipitate can be sintered into solid particles. Then, purified water, a colorant, a water-soluble organic dispersant, a water-soluble polymer stabilizer and a pre-sintered substance are introduced into a ball mill equipped with alumina grinding balls to perform a homogenizing grinding treatment, resulting in a mixed suspension. Thus, the surface tension of the solid particles is removed by the water-soluble organic dispersant, and the solid particles are uniformly dispersed in the solution. The water-soluble polymer stabilizer is used for improving the hardness of the prepared zirconium gem. In addition, the homogenization grinding treatment is performed by a ball mill, so that the colorant, the water-soluble organic dispersant, the water-soluble polymer stabilizer and the pre-sintered substance can be sufficiently and uniformly mixed. Here, the polycrystalline zirconium gem material prepared subsequently can be made to present various colors by using the coloring agent. And finally, carrying out spray drying treatment on the mixed suspension to obtain the polycrystalline zirconium gem material. Therefore, the hardness of the prepared zirconium gem is improved.
With further reference to fig. 2, a flow chart 200 of further embodiments of methods of making polycrystalline zirconium gemstones according to the present disclosure is shown. The preparation method of the polycrystalline zirconium gem comprises the following steps:
And step 204, adding an alkali solution into the mixed solution to completely separate out a solid precipitate.
And step 205, drying and pre-sintering the solid precipitate.
And step 207, carrying out spray drying treatment on the mixed suspension to obtain the polycrystalline zirconium gem material.
In some embodiments, the specific implementation manner and technical effects of steps 201-207 may refer to steps 101-107 in the embodiments corresponding to fig. 1, and are not described herein again.
And 208, adding the colorant into the polycrystalline zirconium gem material for mixing treatment to obtain a mixed polycrystalline zirconium gem material.
In some embodiments, the main body of the polycrystalline zirconium gem preparation method (process machine equipment, where the process machine equipment may include process robots, heating devices (furnaces), cooling devices, spray dryers) may add the above colorants to the above polycrystalline zirconium gem material for mixing treatment, resulting in a mixed polycrystalline zirconium gem material.
In some embodiments, the performing body may heat the mixed polycrystalline zirconium gem material to 1400 ℃ by a heating device and incubate for 60 minutes in response to heating to 1400 ℃. Wherein the heating rate is 10 ℃/min.
And step 210, standing and cooling the mixed polycrystalline zirconium gem material which is kept warm for 60 minutes and is at the temperature of 1400 ℃ to 24-26 ℃ to obtain the polycrystalline zirconium gem.
In some embodiments, the execution body may be configured to allow the mixed polycrystalline zirconium gem material with the temperature of 1400 ℃ after the heat preservation for 60 minutes to stand and cool to 24-26 ℃ to obtain the polycrystalline zirconium gem. Here, the polycrystalline zirconium gem is: the tetragonal phase zirconium dioxide has the density of 5.4-6.2 g/cubic centimeter, the transmittance of less than 30%, the Young modulus of 180-220 Gpa, the Poisson ratio of 0.29-0.34, the propagation rate of sound wave of 5700-6000 m/s and the dielectric loss tangent (Tan delta) of 0 at the wave band of less than 6 GHz.
The related contents of step 208-210 serve as an inventive point of the present disclosure, thereby solving the technical problems mentioned in the background art, namely "the color of the zirconia prepared by the cold crucible method is single". The single color factor of zirconia tends to be as follows: the zirconia prepared by the cold crucible method has a single color. If the above factors are solved, zirconia (zircon stone) of various colors can be prepared. To achieve this effect, the subsequent preparation of zircon stones of various colors is facilitated by adding colorants to the polycrystalline zircon stone powder. The mixed polycrystalline zirconium gem material was then heated to 1400 ℃ and held for 60 minutes in response to heating to 1400 ℃. Thus, the colorant and the zirconium oxide can be sufficiently fused together, so that the color of the zirconium gem cooled subsequently can present various colors. And finally, standing and cooling the mixed polycrystalline zirconium gem material which is kept at the temperature of 1400 ℃ for 60 minutes to 24-26 ℃ to obtain the polycrystalline zirconium gem. Thus, polycrystalline zirconium gemstones of various colors can be produced.
The foregoing description is only exemplary of the preferred embodiments of the disclosure and is illustrative of the principles of the technology employed. It will be appreciated by those skilled in the art that the scope of the invention in the embodiments of the present disclosure is not limited to the specific combination of the above-mentioned features, but also encompasses other embodiments in which any combination of the above-mentioned features or their equivalents is made without departing from the inventive concept as defined above. For example, the above features and (but not limited to) technical features with similar functions disclosed in the embodiments of the present disclosure are mutually replaced to form the technical solution.
Claims (9)
1. A method of preparing a polycrystalline zirconium gemstone, comprising:
adding zirconium oxychloride into purified water to completely dissolve the zirconium oxychloride to obtain a zirconium oxychloride solution;
generating a zirconium sulfate solid based on the zirconium oxychloride solution and sodium sulfate, wherein the mass of the sodium sulfate is 1-2 times of that of the zirconium oxychloride;
dissolving the zirconium sulfate solid in purified water, and adding yttrium chloride and magnesium chloride solution for mixing to obtain a mixed solution;
adding an alkali solution to the mixed solution to completely precipitate a solid precipitate;
drying and pre-sintering the solid precipitate;
introducing purified water, a colorant, a water-soluble organic dispersant, a water-soluble polymer stabilizer and a pre-sintered substance into a ball mill filled with alumina grinding balls to carry out homogenization grinding treatment to obtain a mixed suspension;
and carrying out spray drying treatment on the mixed suspension to obtain the polycrystalline zirconium gem material.
2. The method of claim 1, wherein the generating zirconium sulfate solids based on the zirconium oxychloride solution and sodium sulfate comprises:
adding the sodium sulfate into the zirconium oxychloride solution to obtain a zirconium sulfate mixed solution;
heating the zirconium sulfate mixed solution to 74-76 ℃, and then cooling the zirconium sulfate mixed solution at 74-76 ℃ to 29-31 ℃;
and filtering the zirconium sulfate mixed solution cooled to 29-31 ℃ to obtain a zirconium sulfate solid.
3. The method of claim 1, wherein the adding a base solution to the mixed solution to completely precipitate a solid precipitate comprises:
controlling the temperature range of the mixed solution to be 30-50 ℃, and continuously dripping an alkali solution into the mixed solution and stirring for 20 minutes to obtain a first stirred mixed solution, wherein the pH value of the alkali solution is more than 7 and less than 9, and the stirring speed is 100 revolutions per minute;
controlling the temperature range of the first stirring mixed solution to be 55-75 ℃, and continuously dripping a first alkali solution into the first stirring mixed solution and stirring for 10 minutes to obtain a second stirring mixed solution, wherein the PH value of the first alkali solution is more than or equal to 9 and less than 10, and the stirring rotating speed is 150 revolutions per minute;
controlling the temperature range of the second stirring mixed solution to be 74-76 ℃, and continuously dripping a second alkali solution into the second stirring mixed solution and stirring for 5 minutes to obtain a third stirring mixed solution, wherein the pH value of the second alkali solution is more than or equal to 10 and less than 13, and the stirring speed is 100 revolutions per minute;
and controlling the temperature of the third stirring mixed solution to be 74-76 ℃, and stirring for 30 minutes to completely separate out solid precipitates, wherein the stirring speed is 10 revolutions per minute.
4. The method of claim 1, wherein the drying and pre-sintering the solid precipitate comprises:
carrying out spray drying treatment on the solid precipitate to obtain a dried solid precipitate;
performing the following presintering treatment steps on the dried solid precipitate:
heating the dried solid precipitate to 300 ℃ and holding for 30 minutes in response to heating to 300 ℃, wherein the heating rate is 5 ℃/minute;
heating the dried solid precipitate at 300 ℃ after 30 minutes of incubation to 1300 ℃, and incubating for 60 minutes in response to heating to 1300 ℃, wherein the rate of rise of the heating is 10 ℃/minute;
cooling the dried solid precipitate at 1300 ℃ after 60 minutes of incubation to 1100 ℃, and incubating for 10 minutes in response to cooling to 1100 ℃, wherein the cooling rate of cooling is 10 ℃/minute;
and cooling the dried solid precipitate with the temperature of 1100 ℃ after heat preservation for 10 minutes to 800 ℃, responding to the cooling to 800 ℃, standing and cooling to 24-26 ℃, wherein the cooling rate of the cooling is 20 ℃/minute.
5. The method of claim 1, wherein the pre-sintered mass comprises zirconia; the water-soluble organic dispersant includes one or more of: ammonium citrate polyacrylate, polyethyleneimine; the mass ratio of the water-soluble organic dispersant to the zirconia is as follows: 0.01-1.5: 100.
6. the method of claim 5, wherein the water-soluble polymeric stabilizer comprises one or more of: polyacrylamide, sodium alginate, gelatin, agarose; the mass ratio of the water-soluble polymer stabilizer to the zirconia is as follows: 0.5-4: 100.
7. the method of claim 1, wherein the homogenization milling process is performed by ball milling, wherein the ball milling is performed at a rate of: 60-200 r/min, wherein the ball milling time is as follows: 120-180 minutes.
8. The method according to one of claims 1 to 7, wherein the method further comprises:
adding the colorant into the polycrystalline zirconium gem material for mixing treatment to obtain a mixed polycrystalline zirconium gem material;
heating the mixed polycrystalline zirconium gemstone material to 1400 ℃ and holding for 60 minutes in response to heating to 1400 ℃, wherein the heating rate is 10 ℃/minute;
and standing and cooling the mixed polycrystalline zirconium gem material which is kept at 1400 ℃ for 60 minutes to 24-26 ℃ to obtain the polycrystalline zirconium gem.
9. A polycrystalline zirconium gemstone material prepared by a method for preparing a polycrystalline zirconium gemstone according to any one of claims 1 to 7, the polycrystalline zirconium gemstone material comprising, in mass percent: 70-94% of zirconium oxide, 3-5% of oxide stabilizer and 2-25% of colorant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110750546.9A CN113372113A (en) | 2021-07-01 | 2021-07-01 | Preparation method of polycrystalline zirconium gem |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110750546.9A CN113372113A (en) | 2021-07-01 | 2021-07-01 | Preparation method of polycrystalline zirconium gem |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113372113A true CN113372113A (en) | 2021-09-10 |
Family
ID=77580633
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110750546.9A Pending CN113372113A (en) | 2021-07-01 | 2021-07-01 | Preparation method of polycrystalline zirconium gem |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113372113A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115677346A (en) * | 2022-11-07 | 2023-02-03 | 北京赛乐米克材料科技有限公司 | Preparation method of color zirconium gem ceramic nose pad |
| CN116477941A (en) * | 2023-04-19 | 2023-07-25 | 中物院成都科学技术发展中心 | Artificial jade pottery and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1987007885A1 (en) * | 1986-06-17 | 1987-12-30 | Commonwealth Scientific And Industrial Research Or | Preparation of hydrolysed zirconium salt precursors and high purity zirconia |
| CN1051713A (en) * | 1989-11-11 | 1991-05-29 | 海尔母特·沙尔福 | Zirconium dioxide powder and preparation thereof, application with and sintered compact |
| CN101844920A (en) * | 2010-05-13 | 2010-09-29 | 清华大学 | Preparation method of colored zirconia ceramics |
| CN102757222A (en) * | 2012-07-20 | 2012-10-31 | 株洲市创锐高强陶瓷有限公司 | Composite stable microcrystal zirconium oxide ceramic mixed powder and manufacturing process |
| CN107365149A (en) * | 2017-09-07 | 2017-11-21 | 张家港市六福新材料科技有限公司 | A kind of preparation method of zirconium oxide magnesia ceramics material |
| CN109678500A (en) * | 2019-01-30 | 2019-04-26 | 广州德隆宝环保科技有限公司 | Yttrium stable zirconium oxide ceramic powders and its preparation method and application |
| CN109721357A (en) * | 2019-03-15 | 2019-05-07 | 中南大学 | A kind of Zirconium oxide powder and its preparation method and application that the nanometer yttrium that monodisperse granularity is controllable is stable |
| CN112851342A (en) * | 2021-02-03 | 2021-05-28 | 中新棠国业(苏州)医疗科技有限公司 | Zirconia ceramic material and preparation method and application thereof |
-
2021
- 2021-07-01 CN CN202110750546.9A patent/CN113372113A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1987007885A1 (en) * | 1986-06-17 | 1987-12-30 | Commonwealth Scientific And Industrial Research Or | Preparation of hydrolysed zirconium salt precursors and high purity zirconia |
| CN1051713A (en) * | 1989-11-11 | 1991-05-29 | 海尔母特·沙尔福 | Zirconium dioxide powder and preparation thereof, application with and sintered compact |
| CN101844920A (en) * | 2010-05-13 | 2010-09-29 | 清华大学 | Preparation method of colored zirconia ceramics |
| CN102757222A (en) * | 2012-07-20 | 2012-10-31 | 株洲市创锐高强陶瓷有限公司 | Composite stable microcrystal zirconium oxide ceramic mixed powder and manufacturing process |
| CN107365149A (en) * | 2017-09-07 | 2017-11-21 | 张家港市六福新材料科技有限公司 | A kind of preparation method of zirconium oxide magnesia ceramics material |
| CN109678500A (en) * | 2019-01-30 | 2019-04-26 | 广州德隆宝环保科技有限公司 | Yttrium stable zirconium oxide ceramic powders and its preparation method and application |
| CN109721357A (en) * | 2019-03-15 | 2019-05-07 | 中南大学 | A kind of Zirconium oxide powder and its preparation method and application that the nanometer yttrium that monodisperse granularity is controllable is stable |
| CN112851342A (en) * | 2021-02-03 | 2021-05-28 | 中新棠国业(苏州)医疗科技有限公司 | Zirconia ceramic material and preparation method and application thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115677346A (en) * | 2022-11-07 | 2023-02-03 | 北京赛乐米克材料科技有限公司 | Preparation method of color zirconium gem ceramic nose pad |
| CN115677346B (en) * | 2022-11-07 | 2023-09-12 | 北京赛乐米克材料科技有限公司 | Preparation method of colored zirconium precious stone ceramic nose pad |
| CN116477941A (en) * | 2023-04-19 | 2023-07-25 | 中物院成都科学技术发展中心 | Artificial jade pottery and preparation method thereof |
| CN116477941B (en) * | 2023-04-19 | 2024-02-23 | 中物院成都科学技术发展中心 | Artificial jade pottery and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113372113A (en) | Preparation method of polycrystalline zirconium gem | |
| CN106297904A (en) | UO2the preparation method of SiC fuel pellet and use the UO that this preparation method makes2siC fuel pellet | |
| CN108409676A (en) | A method of control NTO crystal morphologies and granularity | |
| CN102659392A (en) | Preparation method of calcined alumina powder for black ceramics | |
| CN104072112B (en) | A kind of rare earth coated aluminum oxide base ceramic core | |
| CN110016322A (en) | Micron order magnetic coupling abrasive material and water-base magnetic rheology polishing liquid | |
| CN113563071A (en) | Preparation method of blue zirconia ceramic | |
| CN108929039A (en) | A kind of crystalline glaze glaze | |
| CN109336590A (en) | Magnesia partial stabilized zirconia, magnesia partial stabilized zirconia ceramic and its preparation method and application | |
| CN104072137A (en) | Ceramic core for water pump impeller | |
| CN116535196A (en) | Preparation method and application of alumina ceramic | |
| CN104128556A (en) | Easily removable and collapsible inorganic ceramic core | |
| CN104129975A (en) | Rare earth coated calcium oxide based ceramic core | |
| CN106006701B (en) | A kind of preparation method of micrometer-submicrometer grade RE oxide powder | |
| CN108997774A (en) | The manufacturing method of organic cobalt complex | |
| CN109574661A (en) | A kind of preparation method and application of barium zirconate ceramic core | |
| CN101575209A (en) | Textured ceramic niobate template material with controllable thickness and radial dimension and preparation method thereof | |
| CN110105792A (en) | A kind of nanometer transparent ferric oxide red colorant and preparation method thereof | |
| JP2001348220A (en) | Spherical leucite crystal and manufacturing method thereof | |
| CN116791203A (en) | Method for preparing electro-optic crystal growth raw material of oxygen titanium rubidium phosphate by wet chemical coprecipitation method | |
| CN108640615A (en) | Heat discoloration mortar and preparation method thereof | |
| JPS6317297A (en) | Production of ruby single crystal | |
| CN110128013B (en) | Firing method of colored glass for decoration | |
| CN115763953A (en) | Method for preparing LLZO solid electrolyte by using self-propagating combustion method | |
| JPS59152289A (en) | Production of star blue sapphire |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210910 |
|
| RJ01 | Rejection of invention patent application after publication |