CN112850729B - Ce 3+ Preparation method of doped lithium disilicate nanoparticles - Google Patents

Ce 3+ Preparation method of doped lithium disilicate nanoparticles Download PDF

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CN112850729B
CN112850729B CN202110118516.6A CN202110118516A CN112850729B CN 112850729 B CN112850729 B CN 112850729B CN 202110118516 A CN202110118516 A CN 202110118516A CN 112850729 B CN112850729 B CN 112850729B
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lithium disilicate
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doped lithium
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CN112850729A (en
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张辉
陈文革
杨涛
钱颖
杨雅娜
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Xian University of Technology
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
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    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C01B33/32—Alkali metal silicates
    • C01B33/325—After-treatment, e.g. purification or stabilisation of solutions, granulation; Dissolution; Obtaining solid silicate, e.g. from a solution by spray-drying, flashing off water or adding a coagulant
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    • C01—INORGANIC CHEMISTRY
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    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract

The invention discloses Ce 3+ The preparation method of doped lithium disilicate micro-nano powder comprises the steps of firstly, ce (NO) 3 ) 3 ·6H 2 Dissolving O in deionized water, adding TEOS, stirring, and adding LiOH-H 2 Adding O into the mixed solution of cerium nitrate and ethyl orthosilicate, and magnetically stirring until LiOH & H 2 And (3) completely dissolving O to obtain a mixed solution, pouring the mixed solution into a polytetrafluoroethylene inner container, sealing a stainless steel reaction kettle, carrying out hydrothermal reaction to obtain a light yellow precipitate, and carrying out suction filtration, washing and drying on the precipitate to obtain uniform lithium disilicate micro-nano powder. The method has the advantages of low equipment requirement, simple operation, low raw material price, adjustable and easily-controlled reaction parameter range and high product yield, and the prepared lithium disilicate micro-nano powder has controllable micro-porous structure and uniform particle size, and is suitable for large-scale industrial production and commercial popularization.

Description

Ce 3+ Preparation method of doped lithium disilicate nanoparticles
Technical Field
The invention belongs to the technical field of preparation of inorganic micro-nano powder, and relates to Ce 3+ A preparation method of doped lithium disilicate nano particles.
Background
Lithium disilicate (Li) 2 Si 2 O 5 ) The material is mainly used as a biomedical material (such as an all-ceramic dental lithium disilicate glass-ceramic material) for research due to the characteristics of excellent physicochemical, optical and mechanical properties, good thermal stability and the like. Meanwhile, because the lithium disilicate has special biological activity and nontoxicity, the lithium disilicate can be used as a chemical adsorption material, an anti-corrosion coating and the like, and has potential application value in the field of environmental protection. However, there are few reports of intensive research on such multifunctional lithium disilicate materials, which has influenced the development of lithium disilicate in more fields. Therefore, the method has important significance in the deep research and study on the preparation and the performance of the environment-friendly lithium disilicate material.
At present, the traditional processes such as a reaction sintering method, a sol-gel method and the like have the problems of low yield, uneven quality and the like of the prepared lithium disilicate powder, and the application of the lithium disilicate powder in the fields of adsorption, high-performance materials and the like is greatly restricted. In recent years, with the development of synthesis processes and micro-analysis techniques, three-dimensional micro-nano structure materials assembled by one-dimensional/two-dimensional nano basic units have controllable physicochemical, electrical, optical and other properties due to the characteristics of anisotropy, multiple three-dimensional forms, overall high specific surface area and the like of the assembled units, become an important research direction of multifunctional three-dimensional micro-nano materials, and provide powerful theoretical support for researchers to research structure materials with different micro-form particles.
In the existing research, a hydrothermal reaction technology is utilized to synthesize two-dimensional lithium disilicate nanosheets and three-dimensional beam-shaped lithium disilicate powder, although great breakthrough is made in process, dimension and dimension, the regulation and control ranges of purity, dimension and dimension are still narrow, and the form regulation and control of the lithium disilicate micro-nano powder is not realized. Therefore, how to prepare the lithium disilicate micro-nano powder with controllable morphological structure (structural parameters such as particle morphology, size and the like) by a simple and effective method is still a prerequisite to be urgently solved in basic application research.
Disclosure of Invention
The object of the present invention is to provide a Ce 3+ The preparation method of the doped lithium disilicate nano particles solves the problem that the shape regulation of lithium disilicate micro-nano powder is not realized in the prior art.
The technical scheme adopted by the invention is that Ce 3+ The preparation method of the doped lithium disilicate nano particles is implemented according to the following steps:
step 1, adding Ce (NO) 3 ) 3 ·6H 2 Adding O into deionized water, and stirring to obtain Ce (NO) 3 ) 3 ·6H 2 Completely dissolving O to obtain a transparent cerous nitrate aqueous solution;
step 2, weighing TEOS, dropwise adding the TEOS into the cerium nitrate aqueous solution prepared in the step 1, and continuously performing magnetic stirring after dropwise adding is completed to obtain a cerium nitrate-tetraethoxysilane mixed solution;
step 3, weighing LiOH. H 2 O is poured into the mixed solution of cerium nitrate and ethyl orthosilicate obtained in the step 2 to lead LiOH.H 2 O is overFully dissolving to obtain a mixed solution;
step 4, pouring the mixed solution obtained in the step 3 into a polytetrafluoroethylene inner container, and carrying out sealed reaction in a stainless steel reaction kettle to obtain a precipitate;
and 5, carrying out suction filtration on the precipitate prepared in the step 4, washing the precipitate for 3-6 times by using distilled water and alcohol respectively, removing residual solution impurities to obtain a filter cake, carrying out heat preservation and drying on the filter cake, removing water molecules and alcohol molecules to obtain powder, and sieving the faint yellow powder in a screen of more than 1000 meshes.
Step 6, manually grinding and re-screening the large particle aggregates screened out in the step 5, and repeating the step 5 until all the large particle aggregates are screened to obtain Ce 3+ Doped lithium disilicate nanoparticles.
The invention is also characterized in that:
the magnetic stirring time of the step 1 is 10-15 min, and the stirring speed is 800-1500r/min.
The dripping time of the step 2 is 5-10 min, the magnetic stirring time is 15-40 min, and the speed is 800-1500r/min.
Ce in the mixed solution of step 3 3+ The mol ratio of Li to Li is 0.005-0.03, the mol ratio of Li to Si is 0.8-1, the magnetic stirring time is 15-30 min, and the magnetic stirring speed is 800-1500r/min.
The volume filling degree of the polytetrafluoroethylene inner container in the step 4 is 65-75%, the reaction temperature is 150-180 ℃, the reaction time is 24-48 h, and the solid content of the raw materials in the mixed solution is 200-400 g/L.
In the step 5, the filter cake is dried at the temperature of 80-100 ℃ for 12-24 h.
The invention has the beneficial effects that:
1. ce of the invention 3+ The preparation method of the doped lithium disilicate micro-nano powder adopts deionized water as a unique solvent, is easy to clean and exchange in the later separation process and has no pollution to the environment; the adopted raw materials are Tetraethoxysilane (TEOS) and cerous nitrate hexahydrate (Ce (NO) 3 ) 3 ·6H 2 O), lithium hydroxide monohydrate (LiOH. H) 2 O) avoiding the introduction or generation thereofOther impurities and harmful substances.
2. The invention adopts a hydrothermal reaction synthesis process, takes a stainless steel reaction kettle as a shell, is safe in sealing, does not overflow harmful substances, has low reaction temperature, saves energy and protects environment.
3. By adjusting Ce in the invention 3+ The doping molar ratio can realize the regulation and control of the three-dimensional morphology structure of the lithium disilicate micro-nano powder; the obtained lithium disilicate micro-nano powder is uniform in shape and size, is beneficial to dispersion, and can meet the technical application requirements.
Drawings
FIG. 1 is a Ce of the present invention 3+ Different Ce of doped lithium disilicate nanoparticle preparation method 3+ A picture of the shape of lithium disilicate micro-nano powder prepared by doping amount hydrothermal preparation;
FIG. 2 is a Ce of the present invention 3+ Ce of preparation method of doped lithium disilicate nano-particles 3+ XRD pattern of lithium disilicate doped micro-nano powder.
FIG. 3 is a Ce of the present invention 3+ Ce of preparation method of doped lithium disilicate nano-particles 3+ And (3) element distribution diagram of the doped lithium disilicate micro-nano powder.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
Ce of the invention 3+ The preparation method of the doped lithium disilicate nano particles is implemented according to the following steps:
ce 3+ The preparation method of the doped lithium disilicate nano particles is implemented according to the following steps:
step 1, adding Ce (NO) 3 ) 3 ·6H 2 Adding O into deionized water, magnetically stirring for 10-15 min at 800r/min to obtain Ce (NO) 3 ) 3 ·6H 2 Completely dissolving O to obtain a transparent cerous nitrate aqueous solution;
step 2, weighing TEOS, dropwise adding the TEOS into the transparent cerium nitrate aqueous solution prepared in the step 1 within 5min, and then continuing to stir by magnetic force at the speed of 800r/min for 15min to obtain a uniform cerium nitrate-ethyl orthosilicate mixed solution;
step 3, weighing LiOH. H 2 O is poured into the mixed solution of cerium nitrate and ethyl orthosilicate obtained in the step 2 to ensure that Ce is added 3+ The mol ratio of Li to Li is 0.005, the mol ratio of Li to Si is 0.8, the mixture is stirred for 15min by magnetic force, the stirring speed is 800r/min, and the mixture is completely dissolved to obtain uniform mixed solution;
step 4, pouring the mixed solution obtained in the step 3 into a polytetrafluoroethylene inner container, controlling the volume filling degree of the inner container to be 65%, sealing the stainless steel reaction kettle for reaction for 24 hours at 180 ℃, and obtaining light yellow precipitate, wherein the solid content of the raw materials in the reaction solution is 200 g/L;
and 5, carrying out suction filtration on the light yellow precipitate prepared in the step 4, washing the light yellow precipitate for 3 times by using distilled water and alcohol respectively, removing residual solution impurities to obtain a light yellow filter cake, carrying out heat preservation and drying on the filter cake at the temperature of 80 ℃ for 12 hours, removing water molecules and alcohol molecules to obtain light yellow powder, sieving the light yellow powder in a 1000-mesh sieve, and sieving aggregates which may be aggregated during drying.
Step 6, manually grinding and re-screening the large particle aggregates screened out in the step 5, and repeating the step 5 until all the large particle aggregates are screened to obtain Ce 3+ Doped lithium disilicate nanoparticles.
The following expressions may be used:
in the invention of Ce 3+ The preparation method of the doped lithium disilicate nano-particles comprises the following steps:
adopt magnetic stirring, its advantage lies in: the magnetic stirring operation is simple, the method does not need sealing operation, has low operation requirement on the early stage of reaction, and is convenient for industrial production.
The step 1 sets the molar ratio of Li to Si to be 0.8-1, and has the advantages that: can simultaneously ensure the high purity and the high crystallinity of the lithium disilicate product.
Step 1 setting up Ce 3+ The mol ratio of the Li to the Li is 0.005-0.03, and the method has the advantages that: on the premise of ensuring a high-purity product, the microscopic morphology of the lithium disilicate can be regulated and controlled, and the scale and the dimensionality of the product can be effectively regulated and controlled.
The invention has wide range of raw material proportion and hydrothermal filling degree, and has the advantages that: the method has the advantage of easy control for the subsequent large-scale production.
Step 5 adopts the suction filtration process to wash through pure water and alcohol, and has the advantages that: the residual solvent in the reaction and unreacted ions adsorbed on the product can be removed, and meanwhile, hard agglomeration in the subsequent drying process can be avoided, and the dispersibility of the product is improved.
And 5, sieving by adopting a small-mesh sieve (more than 1000 meshes) with the following functions: the method can effectively screen out large-particle aggregates possibly existing in the drying process, and prevent the aggregates from occurring in the subsequent adsorption application process.
In conclusion, the method has the advantages of low equipment requirement, simplicity in operation, low raw material price, adjustable and easily-controlled reaction parameter range and high product yield, and the prepared lithium disilicate micro-nano powder has controllable micro-porous structure and uniform particle size, and is suitable for large-scale industrial production and commercial popularization.
Example 2
Ce of the invention 3+ The preparation method of the doped lithium disilicate nano particles is implemented according to the following steps:
ce 3+ The preparation method of the doped lithium disilicate nano particles is implemented according to the following steps:
step 1, adding Ce (NO) 3 ) 3 ·6H 2 Adding O into deionized water, magnetically stirring at 950r/min for 12min to obtain Ce (NO) 3 ) 3 ·6H 2 Completely dissolving O to obtain a transparent cerous nitrate aqueous solution;
step 2, weighing TEOS, dropwise adding the TEOS into the transparent cerium nitrate aqueous solution prepared in the step 1 within 6min, and then continuing to stir by magnetic force at the speed of 950r/min for 25min to obtain a uniform cerium nitrate-tetraethoxysilane mixed solution;
step 3, weighing LiOH. H 2 O is poured into the mixed solution of cerium nitrate and ethyl orthosilicate obtained in the step 2 to ensure that Ce is added 3+ The mol ratio of Li to Li is 0.01, the mol ratio of Li to Si is 1, the mixture is magnetically stirred for 20min at the stirring speedThe degree is 950r/min, so that the mixture is completely dissolved to obtain a uniform mixed solution;
step 4, pouring the mixed solution obtained in the step 3 into a polytetrafluoroethylene inner container, controlling the volume filling degree of the inner container to be 70%, carrying out sealed reaction in a stainless steel reaction kettle, reacting for 48 hours at 150 ℃, and obtaining light yellow precipitate, wherein the solid content of the raw materials in the reaction solution is 280 g/L;
and 5, carrying out suction filtration on the light yellow precipitate prepared in the step 4, washing the light yellow precipitate for 3 times by using distilled water and alcohol respectively, removing residual solution impurities to obtain a light yellow filter cake, carrying out heat preservation and drying on the filter cake at 100 ℃ for 24 hours, removing water molecules and alcohol molecules to obtain light yellow powder, sieving the light yellow powder in a 1000-mesh sieve, and sieving aggregates which may be aggregated during drying.
Step 6, manually grinding and re-screening the large particle aggregates screened out in the step 5, and repeating the step 5 until all the large particle aggregates are screened to obtain Ce 3+ Doped lithium disilicate nanoparticles.
Example 3
Ce of the invention 3+ The preparation method of the doped lithium disilicate nano particles is implemented according to the following steps:
ce 3+ The preparation method of the doped lithium disilicate nano particles is implemented according to the following steps:
step 1, adding Ce (NO) 3 ) 3 ·6H 2 Adding O into deionized water, magnetically stirring at 1000r/min for 15min to obtain Ce (NO) 3 ) 3 ·6H 2 Completely dissolving O to obtain a transparent cerous nitrate aqueous solution;
step 2, weighing TEOS, dropwise adding the TEOS into the transparent cerium nitrate aqueous solution prepared in the step 1 within 8min, and then continuing to stir by magnetic force at the speed of 1000r/min for 30min to obtain a uniform cerium nitrate-ethyl orthosilicate mixed solution;
step 3, weighing LiOH. H 2 O is poured into the mixed solution of cerium nitrate and ethyl orthosilicate obtained in the step 2 to ensure that Ce is added 3+ The mol ratio of Li to Li is 0.03, the mol ratio of Li to Si is 1, the mixture is magnetically stirred for 30min, and the stirring speed is 1000r/min, so that the mixture is completely dissolved to obtain a uniform mixed solution;
step 4, pouring the mixed solution obtained in the step 3 into a polytetrafluoroethylene inner container, controlling the volume filling degree of the inner container to be 70%, sealing the stainless steel reaction kettle for reaction, reacting for 35 hours at 180 ℃, and obtaining light yellow precipitate, wherein the solid content of the raw materials in the reaction solution is 360 g/L;
and 5, carrying out suction filtration on the light yellow precipitate prepared in the step 4, washing the light yellow precipitate for 5 times by using distilled water and alcohol respectively, removing residual solution impurities to obtain a light yellow filter cake, carrying out heat preservation and drying on the filter cake at 90 ℃ for 18h, removing water molecules and alcohol molecules to obtain light yellow powder, sieving the light yellow powder in a screen with the mesh size of more than 1000, and screening aggregates which may be aggregated during drying.
Step 6, manually grinding and re-screening the large particle aggregates screened out in the step 5, and repeating the step 5 until all the large particle aggregates are screened to obtain Ce 3+ Doped lithium disilicate nanoparticles.
Example 4
Ce of the invention 3+ The preparation method of the doped lithium disilicate nano particles is implemented according to the following steps:
ce 3+ The preparation method of the doped lithium disilicate nano particles is implemented according to the following steps:
step 1, adding Ce (NO) 3 ) 3 ·6H 2 Adding O into deionized water, magnetically stirring for 15min at 1500r/min to obtain Ce (NO) 3 ) 3 ·6H 2 Completely dissolving O to obtain a transparent cerous nitrate aqueous solution;
step 2, weighing TEOS, dropwise adding the TEOS into the transparent cerium nitrate aqueous solution prepared in the step 1 within 10min, and then continuing to stir by magnetic force at the speed of 1500r/min for 40min to obtain a uniform cerium nitrate-ethyl orthosilicate mixed solution;
step 3, weighing LiOH. H 2 O is poured into the mixed solution of cerium nitrate and ethyl orthosilicate obtained in the step 2 to lead Ce to be 3+ The mol ratio of Li to Li is 0.02, the mol ratio of Li to Si is 1, the magnetic stirring is carried out for 40min, and the stirring speed is 1500r/min to completely dissolve the mixture to obtain a uniform mixed solution;
step 4, pouring the mixed solution obtained in the step 3 into a polytetrafluoroethylene inner container, controlling the volume filling degree of the inner container to be 75%, sealing the stainless steel reaction kettle for reaction, reacting for 48 hours at 180 ℃, and obtaining light yellow precipitate, wherein the solid content of the raw materials in the reaction solution is 400 g/L;
and 5, carrying out suction filtration on the light yellow precipitate prepared in the step 4, washing the light yellow precipitate for 3-6 times by using distilled water and alcohol respectively, removing residual solution impurities to obtain a light yellow filter cake, carrying out heat preservation and drying on the filter cake at the temperature of 80 ℃ for 24 hours, removing water molecules and alcohol molecules to obtain light yellow powder, sieving the light yellow powder in a screen of more than 1000 meshes, and screening out aggregates which may be aggregated during drying.
Step 6, manually grinding and re-screening the large particle aggregates screened out in the step 5, and repeating the step 5 until all the large particle aggregates are screened to obtain Ce 3+ Doped lithium disilicate nanoparticles.
According to the conclusion made by supplementing the description of the four embodiments, the invention has the advantages that:
as can be seen from FIGS. 1 (a) and (b), the typical lithium disilicate micro-nano powder obtained by the invention has different Ce 3+ The doping amount can regulate and control the microscopic morphology of the lithium disilicate assembly unit, and the lithium disilicate assembly unit is respectively a nearly rectangular two-dimensional nano sheet (Ce) 3+ /Li = 0.01) and a nearly semicircular two-dimensional nanosheet (Ce) 3+ /Li = 0.005). Moreover, the particles have complete integral structure and uniform appearance and size, are all flower-shaped three-dimensional structures with the size of about 1 mu m, and show that the particles have good crystal form integrity and micro-parameter adjustability such as dimension and dimensionality.
As can be seen from FIG. 2, no other impurity phase is observed in XRD, which indicates that the crystallinity and purity of the crystal phase of the lithium disilicate micro-nano powder are high, and further indicates that Ce is also included 3+ The lithium disilicate crystal prepared by the doping hydrothermal method has good growth and development.
As can be seen from FIG. 3, the distribution of elements in the lithium disilicate nanoflower structure indicates that Ce is present 3+ Uniformly distributed in the particle structure, further illustrates Ce 3+ The morphological control function of (2) verifies the above-mentioned microscopic morphological adjustability.

Claims (5)

1. Ce 3+ The preparation method of the doped lithium disilicate nano particles is characterized by comprising the following steps:
step 1, adding Ce (NO) 3 ) 3 ·6H 2 Adding O into deionized water, and stirring to obtain Ce (NO) 3 ) 3 ·6H 2 Completely dissolving O to obtain a transparent cerous nitrate aqueous solution;
step 2, weighing TEOS, dropwise adding the TEOS into the cerium nitrate aqueous solution prepared in the step 1, and continuously performing magnetic stirring after dropwise adding is completed to obtain a cerium nitrate-tetraethoxysilane mixed solution;
step 3, weighing LiOH. H 2 O is poured into the mixed solution of cerium nitrate and ethyl orthosilicate obtained in the step 2 to lead LiOH.H 2 Completely dissolving O to obtain a mixed solution;
step 4, pouring the mixed solution obtained in the step 3 into a polytetrafluoroethylene inner container, and carrying out sealed reaction in a stainless steel reaction kettle to obtain a precipitate;
step 5, carrying out suction filtration on the precipitate prepared in the step 4, washing the precipitate with distilled water and alcohol for 3 to 6 times respectively, removing impurities in the residual solution to obtain a filter cake, carrying out heat preservation and drying on the filter cake, removing water molecules and alcohol molecules to obtain powder, and sieving the faint yellow powder in a screen with the mesh size of more than 1000 meshes;
step 6, manually grinding and re-screening the large particle aggregates screened out in the step 5, and repeating the step 5 until all the large particle aggregates are screened to obtain Ce 3+ Doping lithium disilicate nanoparticles;
ce in the mixed solution of the step 3 3+ The mol ratio of Li to Li is 0.005 to 0.03, the mol ratio of Li to Si is 0.8 to 1, the magnetic stirring time is 15 to 30min, and the magnetic stirring speed is 800 to 1500r/min.
2. Ce according to claim 1 3+ The preparation method of the doped lithium disilicate nano-particles is characterized in that the magnetic stirring time in the step 1 is 10 to 15min,the stirring speed is 800-1500r/min.
3. Ce according to claim 1 3+ The preparation method of the doped lithium disilicate nanoparticles is characterized in that the dropping time of the step 2 is 5-10min, the magnetic stirring time is 15-40min, and the speed is 800-1500r/min.
4. Ce according to claim 1 3+ The preparation method of the doped lithium disilicate nano-particles is characterized in that the volume filling degree of the polytetrafluoroethylene inner container in the step 4 is 65-75%, the reaction temperature is 150-180 ℃, the reaction time is 24-48 h, and the solid content of the raw materials in the mixed solution is 200-400 g/L.
5. Ce according to claim 4 3+ The preparation method of the doped lithium disilicate nano-particles is characterized in that the heat preservation drying temperature of the filter cake in the step 5 is 80-100 ℃, and the heat preservation drying time is 12-24 hours.
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