CN108560052A - A kind of preparation method and applications of six side's aluminium oxide of monocrystalline - Google Patents
A kind of preparation method and applications of six side's aluminium oxide of monocrystalline Download PDFInfo
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- CN108560052A CN108560052A CN201810385666.1A CN201810385666A CN108560052A CN 108560052 A CN108560052 A CN 108560052A CN 201810385666 A CN201810385666 A CN 201810385666A CN 108560052 A CN108560052 A CN 108560052A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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- General Chemical & Material Sciences (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a kind of preparation methods of six side's aluminium oxide of monocrystalline, including：(1) crystal form agent is added in aluminum salt solution；(2) under agitation, precipitant solution is added drop-wise in the solution that step (1) obtains, lasting to stir, then control ph is added fused salt and is uniformly mixed, be prepared into gel mixture 9 10；(3) high-temperature calcination is carried out after drying gel mixture；(4) the cooling, washing by the mixture after calcining, through filtering, being dried to obtain six side's alumina particle of monocrystalline.Application of the six side's aluminium oxide of monocrystalline and six side's aluminium oxide of the monocrystalline being prepared the invention further relates to the method as lacquer painting inlaid material.Crystal form agent is added by raw material of aluminium salt in the present invention, can promote the regular growth of aluminium oxide, using molten-salt growth method, grain size is prepared in 40 60um, thickness is six side's alumina particle of monocrystalline of 1 4um, is embedded in that starlight in lacquer painting is bright, the unique artistic effect with agile crystal.
Description
Technical field
The present invention relates to the preparation method and applications of six side's aluminium oxide of monocrystalline, and in particular to a kind of six side's aluminium oxide of monocrystalline
Preparation method and by this method prepare six side's aluminium oxide of monocrystalline and six side's aluminium oxide of the monocrystalline inlayed as lacquer painting
The application of material.
Background technology
Chinese lacquer painting be one in contemporary painting circles it is newborn draw kind, be using natural lacquer as the painting creation of main material,
Double attribute with drawing and technique, with its unique esthetics idea based on painting circles.This unique esthetics idea is except next
Its inlaid material is also relied on from outside the characteristic of lacquer.Inlaid material used needs certain hardness on lacquer painting, wear-resisting, changes
The characteristics such as stability is good are learned, there are commonly the precious metal materials such as gold, silver, the shells material such as green snail, abalone shellfish, thin slice eggshells
And the inorganic non-metallic materials such as seleced jade.These materials paint, which is picked up, is attached to the required position of picture, in conjunction with other
Decoration technology can generate the unique effect such as different material textures, texture, color after coating with lacquer paint grinding.
Tabular alumina object is mutually α-Al2O3, also referred to as corundum, Mohs' hardness 9 are the height that hardness is only second to diamond
Hardness substance, wearability is good, high temperature resistant and stable chemical performance.However presently disclosed tabular alumina is mainly used in polishing
The tabular alumina grain size of industry and pearly-lustre industry, preparation is smaller (about 10um), it is difficult to apply, present in lacquer painting inlaid material
Artistic effect.
Invention content
An object of the present invention be to provide it is a kind of have smooth larger particle and certain thickness, surface, good dispersion,
Shape is six side's aluminium oxide of monocrystalline of regular shape.
It is a further object of the present invention to provide the preparation methods of six side's aluminium oxide of above-mentioned monocrystalline.
Another object of the present invention is to provide application of the six side's aluminium oxide of above-mentioned monocrystalline as lacquer painting inlaid material.
Present invention firstly provides a kind of preparation methods of six side's aluminium oxide of monocrystalline, include the following steps：
(1) crystal form agent is added in aluminum salt solution, stirs evenly；
(2) under agitation, precipitant solution is added drop-wise in the solution that step (1) obtains, is then persistently stirred, controlled
PH value processed is eventually adding fused salt and is uniformly mixed, be prepared into gel mixture in 9-10；
(3) high-temperature calcination is carried out after drying gel mixture, temperature is 1150-1350 DEG C, time 2-8h；
(4) mixture after calcining is cooled to room temperature, is then washed with water, fused salt is removed, through filtering, being dried to obtain list
Brilliant six side's alumina particles.
Further：
The aluminum salt solution includes aluminum sulfate solution.The mass concentration of the aluminium salt is 20~60%.
The precipitant solution includes sodium hydroxide solution or sodium carbonate liquor.The mass concentration of the precipitating reagent be 15~
40%.
The crystal form agent is the mixture of one or both of zirconates, molybdate；The additive amount of the crystal form agent is pressed
The amount of finally obtained aluminium oxide is calculating standard, and weight ratio is 0.05~5%, preferably 0.1~3%.Pass through the crystalline substance
The selection of the dosage of type agent can improve the granule-morphology of tabular alumina, make it have than more complete six squares feature.
The zirconates includes zirconium fluoride, zirconium chloride, zirconium nitrate.
The molybdate includes sodium molybdate, potassium molybdate, ammonium phosphomolybdate.
The fused salt is the mixture of one or both of sylvite, sodium salt.It is highly preferred that the sylvite is potassium sulfate,
The sodium salt is sodium sulphate.
The present invention also provides six side's aluminium oxide of monocrystalline, grain size 40-60um, thickness made from above-mentioned preparation method to be
1-4um。
The present invention finally additionally provides application of the six side's aluminium oxide of the monocrystalline as lacquer painting inlaid material.
The invention has the advantages that：Crystal form agent is added by raw material of aluminium salt in the present invention, can promote the regular growth of aluminium oxide,
Using molten-salt growth method, grain size is prepared in 40-60um, thickness is six side's alumina particle of monocrystalline of 1-4um, is embedded in lacquer painting
Starlight is bright, the unique artistic effect with agile crystal.
Description of the drawings
The present invention is further illustrated in conjunction with the embodiments with reference to the accompanying drawings.
Fig. 1 is the electron micrograph of 1 signle crystal alumina crystal grain shape of embodiment.
Fig. 2 is the X ray diffracting spectrum of 1 signle crystal alumina crystal of embodiment.
Fig. 3 is the monocrystalline hot spot photo of the selective electron diffraction of 1 signle crystal alumina crystal of embodiment.
Fig. 4 is the electron micrograph of 3 signle crystal alumina crystal grain shape of embodiment.
Fig. 5 is the electron micrograph of 3 signle crystal alumina crystal thickness of embodiment.
Fig. 6 is the electron micrograph of 4 signle crystal alumina crystal thickness of embodiment.
Fig. 7 is the electron micrograph of 1 alpha-alumina crystals grain shape of comparative example.
Fig. 8 is the electron micrograph of 1 alpha-alumina crystals thickness of comparative example.
Specific implementation mode
Embodiment 1
1) it takes 100g aluminum sulfate octadecahydrates to be dissolved in 200mL deionized waters, the fluorination zirconium solution of mass percent 1% is added
10mL is made into solution A；37.8g sodium hydroxides are dissolved in 100mL deionized waters, are made into B solution.
2) under agitation (mixing speed 550r/min), above-mentioned B liquid is slowly added in A liquid, is added subsequent
Continuous stirring 25min, control ph is added 40g potassium sulfates and 40g sodium sulfate salts is uniformly mixed 9, to be prepared into gel mixing
Object.
3) crystallization of high temperature resistance high temperature fused salt is put into after drying gel mixture, temperature is 1200 Celsius temperatures, is protected
The warm time is 3h.
4) the mixture cooling water after calcining is washed, removes fused salt, is through filtering, being dried to obtain average grain diameter
Six side's alumina particle of monocrystalline of 50um, thickness are 1~4um.Such as Fig. 1-3.
Embodiment 2
1) it takes 200g aluminum sulfate octadecahydrates to be dissolved in 400mL deionized waters, the Sodium Molybdate Dihydrate of mass percent 5% is added
Solution 18mL, is made into solution A；75.6g sodium hydroxides are dissolved in 200mL deionized waters, are made into B solution.
2) under agitation (mixing speed 550r/min), above-mentioned B liquid is slowly added in A liquid, is added subsequent
Continuous stirring 25min, control ph is added 80g potassium sulfates and 80g sodium sulfate salts is uniformly mixed 9.3, to be prepared into gel mixing
Object.
3) crystallization of high temperature resistance high temperature fused salt is put into after drying gel mixture, temperature is 1250 Celsius temperatures, is protected
The warm time is 2h.
4) the mixture cooling water after calcining is washed, removes fused salt, is through filtering, being dried to obtain average grain diameter
Six side's alumina particle of monocrystalline of 48um, thickness are 1~4um.Such as Fig. 1-3.The XRD spectra of Fig. 2 gives pdf card numbers 46-
1212 corresponding objects are mutually Alpha's aluminium oxide of corundum, i.e. α-Al2O3。
Embodiment 3
1) it takes 100g aluminum sulfate octadecahydrates to be dissolved in 200mL deionized waters, the fluorination zirconium solution of mass percent 1% is added
The Sodium Molybdate Dihydrate solution 8mL of 8mL and mass percent 5%, are made into solution A；37.8g sodium hydroxides are dissolved in 100mL deionizations
In water, it is made into B solution.
2) under agitation (mixing speed 550r/min), above-mentioned B liquid is slowly added in A liquid, is added subsequent
Continuous stirring 25min, control ph is added 40g potassium sulfates and 40g sodium sulfate salts is uniformly mixed 9.5, to be prepared into gel mixing
Object.
3) crystallization of high temperature resistance high temperature fused salt is put into after drying gel mixture, temperature is 1300 Celsius temperatures, is protected
The warm time is 4h.
4) the mixture cooling water after calcining is washed, removes fused salt, is through filtering, being dried to obtain average grain diameter
Six side's alumina particle of monocrystalline of 52um, thickness are 1~4um.Such as Fig. 4-5.
Embodiment 4
1) it takes 200g aluminum sulfate octadecahydrates to be dissolved in 400mL deionized waters, the chlorination zirconium solution of mass percent 5% is added
The Sodium Molybdate Dihydrate solution 12mL of 10mL and 10%, is made into solution A；100.2g sodium carbonate is dissolved in 300mL deionized waters, is made into
B solution.
2) under agitation (mixing speed 550r/min), above-mentioned B liquid is slowly added in A liquid, is added subsequent
Continuous stirring 25min, control ph is added 80g potassium sulfates and 80g sodium sulfate salts is uniformly mixed 9.8, to be prepared into gel mixing
Object.
3) crystallization of high temperature resistance high temperature fused salt is put into after drying gel mixture, temperature is 1280 Celsius temperatures, is protected
The warm time is 8h.
4) the mixture cooling water after calcining is washed, removes fused salt, is through filtering, being dried to obtain average grain diameter
Six side's alumina particle of monocrystalline of 56um, thickness are 1~4um.As shown in Figure 6.
Embodiment 5
1) it takes 100g aluminum sulfate octadecahydrates to be dissolved in 200mL deionized waters, the ammonium phosphomolybdate of mass percent 3% is added
10mL is made into solution A；50.1g sodium carbonate is dissolved in 150mL deionized waters, is made into B solution.
2) under agitation (mixing speed 550r/min), above-mentioned B liquid is slowly added in A liquid, is added subsequent
Continuous stirring 25min, control ph is added 40g potassium sulfates and 40g sodium sulfate salts is uniformly mixed 9, to be prepared into gel mixing
Object.
3) crystallization of high temperature resistance high temperature fused salt is put into after drying gel mixture, temperature is 1240 Celsius temperatures, is protected
The warm time is 4h.
4) the mixture cooling water after calcining is washed, removes fused salt, is through filtering, being dried to obtain average grain diameter
Six side's alumina particle of monocrystalline of 53um, thickness are 1~4um.
The thickness and average grain diameter of the single-crystal platy aluminium oxide prepared in 1 embodiment 1-5 of table
| Crystal form agent % | Thickness um | Average grain diameter um | |
| Embodiment 1 | 0.2 | 1-4 | 50 |
| Embodiment 2 | 1.5 | 1-4 | 48 |
| Embodiment 3 | 1.8 | 1-4 | 52 |
| Embodiment 4 | 2.9 | 1-4 | 56 |
| Embodiment 5 | 1.6 | 1-4 | 53 |
As shown in table 1, prepared in embodiment 1-5 the present invention six side's aluminium oxide of monocrystalline with 1-4um thickness and
The average grain diameter of 40-60um.
Comparative example 1
In addition to 8% titanium sulfate 10mL of use quality percentage replace mass percent 3% ammonium phosphomolybdate 10mL solution with
Outside, alpha-alumina crystals are prepared in a manner of same as Example 5, are seen in the electron micrograph of Fig. 7 and Fig. 8, are made
The average grain diameter of thickness and 12um of the alpha-alumina crystals with 0.2-0.4um.It is concluded that, the crystal with embodiment 1-5
It is irregular compared to the crystal grain shape and too thin, there is smaller average grain diameter, be embedded in lacquer painting and fail that there is spirit
The unique artistic effect of dynamic crystal.
Although specific embodiments of the present invention have been described above, those familiar with the art should manage
Solution, we are merely exemplary described specific embodiment, rather than for the restriction to the scope of the present invention, it is familiar with this
The technical staff in field modification and variation equivalent made by the spirit according to the present invention, should all cover the present invention's
In scope of the claimed protection.
Claims (10)
1. a kind of preparation method of six side's aluminium oxide of monocrystalline, it is characterised in that：Include the following steps：
(1) crystal form agent is added in aluminum salt solution, stirs evenly；
(2) under agitation, precipitant solution is added drop-wise in the solution that step (1) obtains, is then persistently stirred, control pH
Value is eventually adding fused salt and is uniformly mixed, be prepared into gel mixture in 9-10；
(3) high-temperature calcination is carried out after drying gel mixture, temperature is 1150-1350 DEG C, time 2-8h；
(4) mixture after calcining is cooled to room temperature, is then washed with water, fused salt is removed, through filtering, being dried to obtain monocrystalline six
Square alumina particle.
2. the preparation method of six side's aluminium oxide of monocrystalline according to claim 1, it is characterised in that：The aluminum salt solution includes
Aluminum sulfate solution.
3. the preparation method of six side's aluminium oxide of monocrystalline according to claim 1, it is characterised in that：The precipitant solution packet
Include sodium hydroxide solution or sodium carbonate liquor.
4. the preparation method of six side's aluminium oxide of monocrystalline according to claim 1, it is characterised in that：The crystal form agent is zirconium
The mixture of one or both of salt, molybdate；The additive amount of the crystal form agent is by the amount of finally obtained aluminium oxide for based on
Calculation standard, weight ratio are 0.1~3%.
5. the preparation method of six side's aluminium oxide of monocrystalline according to claim 4, it is characterised in that：The zirconates includes fluorination
Zirconium, zirconium chloride, zirconium nitrate.
6. the preparation method of six side's aluminium oxide of monocrystalline according to claim 4, it is characterised in that：The molybdate includes molybdenum
Sour sodium, potassium molybdate, ammonium phosphomolybdate.
7. the preparation method of six side's aluminium oxide of monocrystalline according to claim 1, it is characterised in that：The fused salt be sylvite,
The mixture of one or both of sodium salt.
8. the preparation method of six side's aluminium oxide of monocrystalline according to claim 7, it is characterised in that：The sylvite is sulfuric acid
Potassium, the sodium salt are sodium sulphate.
9. six side's aluminium oxide of monocrystalline that the preparation method as described in claim 1-8 any one obtains, it is characterised in that：The list
The grain size of brilliant six side's aluminium oxide is 40-60um, thickness 1-4um.
10. application of the six side's aluminium oxide of monocrystalline as lacquer painting inlaid material as claimed in claim 9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112442731A (en) * | 2020-11-06 | 2021-03-05 | 昆明理工大学 | Method for directionally regulating and controlling crystal transformation and growth by multiple physical fields |
| CN113930050A (en) * | 2021-11-03 | 2022-01-14 | 安徽工业技术创新研究院六安院 | High-thermal-conductivity low-viscosity epoxy plastic packaging material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112442731A (en) * | 2020-11-06 | 2021-03-05 | 昆明理工大学 | Method for directionally regulating and controlling crystal transformation and growth by multiple physical fields |
| CN113930050A (en) * | 2021-11-03 | 2022-01-14 | 安徽工业技术创新研究院六安院 | High-thermal-conductivity low-viscosity epoxy plastic packaging material and preparation method thereof |
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