CN102863000A - Preparation method of high-purity aluminum oxide for growth of sapphire monocrystalline - Google Patents
Preparation method of high-purity aluminum oxide for growth of sapphire monocrystalline Download PDFInfo
- Publication number
- CN102863000A CN102863000A CN2012103720414A CN201210372041A CN102863000A CN 102863000 A CN102863000 A CN 102863000A CN 2012103720414 A CN2012103720414 A CN 2012103720414A CN 201210372041 A CN201210372041 A CN 201210372041A CN 102863000 A CN102863000 A CN 102863000A
- Authority
- CN
- China
- Prior art keywords
- purity
- raw material
- preparation
- aluminum oxide
- temperature
- 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
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a preparation method of a high-purity aluminum oxide, in particular to a preparation method of high-purity aluminum oxide for growth of sapphire monocrystalline. The method includes: grinding high-purity ammonium aluminum sulfate to obtain ammonium aluminum sulfate precursor powder uniform in particle size, heating according to different temperature sections, pyrolyzing to remove by-products, and sintering to obtain high-purity aluminum oxide uniform in particle size. According to the method, the high-purity ammonium aluminum sulfate is ground to obtain ammonium aluminum sulfate raw material powder, dewatering is completed at a low temperature, ammonia gas is removed at a moderate temperature, the temperature is further increased to enable the raw materials to be decomposed completely, and the high-purity aluminum oxide is obtained by means of sintering at 1000-1050 DEG C. The aluminum oxide prepared by the method is low in pyrolysis temperature and high in purity, tail gases such as SO3 and NH3 can be recovered directly, and consequently environment pollution is reduced, by-products are used reasonably, and production cost is reduced.
Description
Technical field
The present invention relates to a kind of preparation method of high purity aluminium oxide, particularly a kind of preparation method of the high purity aluminium oxide for the growing sapphire monocrystalline.
Background technology
The advantageous properties such as high purity aluminium oxide has high strength, high rigidity, resistance to wears, high temperature resistant, resistance to chemical attack are the important materials of making integrated circuit substrate, light transmission fluorescent tube fluorescent material, function monocrystalline precision meter and aviation optics etc. on the electronic industry.As everyone knows, current led chip adopts sapphire single-crystal as substrate more, and high performance chip is also very harsh to the requirement of substrate, and high-quality substrate is the prerequisite of preparation high performance chips, and this has higher quality and purity with regard to the starting material that require to prepare substrate.Aluminum oxide is as the starting material of preparation sapphire single-crystal, and its purity has direct impact to the crystal mass of sapphire single-crystal.The method for preparing high-purity alpha-alumina also has multiple, such as early stage employing improvement Bayer process, take the meta-aluminic acid ammonium as raw material, obtain high purity aluminium hydroxide through repeatedly desiliconization, deferrization, pyrolytic decomposition supervisor, then obtain high-purity ultra-fine alumina through high-temperature roasting, grinding supervisor.Other two kinds of methods commonly used are Pyrolysis of Ammonium Aluminium Carbonate Hydroxide method (patent CN1448340A) and organoaluminum hydrolysis roasting method (patent CN1342609A) the preparation high purity aluminium oxides take aluminium carbonate ammonium and exsiccated ammonium alum as raw material.But all there are the problems such as the production link that relates in operating procedure complexity, the technique is many in above method.Also having a kind of method relatively commonly used is exsiccated ammonium alum high temperature pyrolysis method, and this method does not need other starting material to participate in, only just can obtain by simple pyrolysis alumina powder jointed, but exist sintering temperature high, contain SO
3The problems such as by product.
Summary of the invention
The objective of the invention is the problem that exists in the existing exsiccated ammonium alum high temperature pyrolysis method, by Optimizing Technical, provide a kind of preparation method of the high purity aluminium oxide that is used for the growing sapphire monocrystalline of more simple, environmental protection.
Technical scheme of the present invention is as follows:
A kind of preparation method of the high purity aluminium oxide for the growing sapphire monocrystalline, it is characterized in that: High-Purity Aluminum Ammonium Sulfate is ground to obtain even-grained exsiccated ammonium alum precursor powder, then pyrolysis is carried out in its minute temperature section heating and removed by product, and obtain high-purity even-grained alumina powder jointed by further sintering.Concrete grammar is:
A, take the High-Purity Aluminum Ammonium Sulfate crystal as raw material, raw material is fully ground, and places in the crucible;
B, raw material and crucible are done as a whole, placed in the process furnace, utilize self crystal water that reactant is dissolved at the 200-300 degree and dewater;
C, the reactant after will dewatering are heated to the 500-600 degree, remove ammonia;
D, reactant further is heated to the 850-950 degree, so that raw material decomposes fully, and sloughs SO in the raw material
3Deng by product;
E, at the 1000-1100 degree with the further sintering of product.
Conversion unit one is connected straight through the water of stainless steel tube with the external world in the whole reaction process of the present invention.
The objective of the invention is to obtain the exsiccated ammonium alum material powder by High-Purity Aluminum Ammonium Sulfate (5N) is ground, then carrying out low temperature dewaters, and under moderate temperature, remove ammonia, the temperature that further raises is decomposed raw material fully, and then has obtained high-purity aluminum oxide by the sintering of 1000-1050 degree.Be about to exsiccated ammonium alum in low, remove under the temperature anhydrate, ammonia, and slightly removing SO under the high-temperature
3, obtained high purity aluminium oxide by sintering at last.In reaction process, by product is directly passed in the water simultaneously, both reduced pollution, can make again by product in water, carry out the acid-base neutralisation reaction, the product of neutralization reaction can also be carried out crystallization, re-use, reached the purpose of achieving many things at one stroke.This method is simple, the advantage that can obtain high-purity alpha-alumina not only, and with to compare sintering temperature with class methods low, the by product environmentally safe, the grinding before the reaction also helps to form the uniform product of particle diameter, is the preparation method of a kind of not only economical and practical but also environmental protection.The aluminum oxide pyrolysis temperature of the present invention's preparation is low, purity is high, and the SO that produces
3, NH
3Tail gas directly reclaims, and has namely reduced pollution to environment, has been that by product is rationally utilized again, has reduced production cost.
Embodiment
Describe in detail below in conjunction with example:
Embodiment 1.
As reaction raw materials, as reaction unit, prepare high purity alumina powder with high temperature Muffle furnace with High-Purity Aluminum Ammonium Sulfate.
At first take by weighing a certain amount of High-Purity Aluminum Ammonium Sulfate, be placed in the mortar, fully grind the exsiccated ammonium alum precursor powder raw material that obtains uniform particle size.Then raw material is transferred in the crucible, and raw material and crucible are made the as a whole high temperature Muffle furnace that places, 220 degree heating 60 minutes, raw material is dissolved in self the crystal water and with crystal water sloughs.Then, stove further is warmed up to 550 degree, maintenance is 1 hour under this temperature, in order to remove the ammonia in the raw material.And then temperature is elevated to 900 degree, insulation is 1 hour under this temperature, so that raw material decomposes fully and with the SO in the raw material
3Remove.At last at 1000 degree with the further sintering of product 1 hour.Conversion unit one is connected straight through the water of stainless steel tube with the external world in the whole reaction process.After reacting end, collect product and products therefrom is carried out structure and purity sign, comprise X-ray diffraction (XRD) θ-2 θ scanning, field emission scanning electron microscope (FESEM) observation, Inductively coupled plasma mass spectrograph (ICP-MS) analysis etc.Wherein the XRD structural analysis shows, products therefrom is mainly α-Al
2O
3, follow simultaneously a small amount of γ-Al
2O
3This mainly causes owing to sintering temperature is not high enough at last, FESEM result shows, the products therefrom epigranular, median size is about 300nm, and SAED the analysis showed that and only contain Al and two kinds of elements of O in the sample, and its ratio of components is substantially near 2:3, further the ICP-MS purity check shows and also only contains Al and two kinds of elements of O in the sample, and purity has reached 99.999%.Above result shows that the aluminum oxide for preparing has the characteristics such as purity is high, particle diameter is even.
Embodiment 2.
As reaction raw materials, as reaction unit, prepare high purity alumina powder with high temperature Muffle furnace with High-Purity Aluminum Ammonium Sulfate.
At first take by weighing a certain amount of High-Purity Aluminum Ammonium Sulfate, be placed in the mortar, fully grind the exsiccated ammonium alum precursor powder raw material that obtains uniform particle size.Then raw material is transferred in the crucible, and raw material and crucible are made the as a whole high temperature Muffle furnace that places, 220 degree heating 60 minutes, raw material is dissolved in self the crystal water and with crystal water sloughs.Then, stove further is warmed up to 530 degree, maintenance is 1 hour under this temperature, in order to remove the ammonia in the raw material.And then temperature is elevated to 900 degree, insulation is 1.5 hours under this temperature, so that raw material decomposes fully and with the SO in the raw material
3Remove.At last at 1030 degree with the further sintering of product 1 hour.Conversion unit one is connected straight through the water of stainless steel tube with the external world in the whole reaction process.After reacting end, collect product and products therefrom is carried out structure and purity sign, comprise X-ray diffraction (XRD) θ-2 θ scanning, field emission scanning electron microscope (FESEM) observation, Inductively coupled plasma mass spectrograph (ICP-MS) analysis etc.Wherein the XRD structural analysis shows, products therefrom is mainly α-Al
2O
3FESEM result shows, the products therefrom epigranular, median size is about 330nm, SAED the analysis showed that and only contains Al and two kinds of elements of O in the sample, its ratio of components is substantially near 2:3, and further the ICP-MS purity check shows and also only contains Al and two kinds of elements of O in the sample, and purity has reached 99.999%.Above result shows that the aluminum oxide for preparing has the characteristics such as purity is high, particle diameter is even.
Embodiment 3.
As reaction raw materials, as reaction unit, prepare high purity alumina powder with high temperature Muffle furnace with High-Purity Aluminum Ammonium Sulfate.
At first take by weighing a certain amount of High-Purity Aluminum Ammonium Sulfate, be placed in the mortar, fully grind the exsiccated ammonium alum precursor powder raw material that obtains uniform particle size.Then raw material is transferred in the crucible, and raw material and crucible are made the as a whole high temperature Muffle furnace that places, 200 degree heating 60 minutes, raw material is dissolved in self the crystal water and with crystal water sloughs.Then, stove further is warmed up to 570 degree, maintenance is 1 hour under this temperature, in order to remove the ammonia in the raw material.And then temperature is elevated to 900 degree, insulation is 1 hour under this temperature, so that raw material decomposes fully and with the SO in the raw material
3Remove.At last at 1050 degree with the further sintering of product 2 hours.Conversion unit one is connected straight through the water of stainless steel tube with the external world in the whole reaction process.After reacting end, collect product and products therefrom is carried out structure and purity sign, comprise X-ray diffraction (XRD) θ-2 θ scanning, field emission scanning electron microscope (FESEM) observation, Inductively coupled plasma mass spectrograph (ICP-MS) analysis etc.Wherein the XRD structural analysis shows, products therefrom is mainly α-Al
2O
3FESEM result shows, the products therefrom epigranular, median size is about 380nm, SAED the analysis showed that and only contains Al and two kinds of elements of O in the sample, its ratio of components is substantially near 2:3, and further the ICP-MS purity check shows and also only contains Al and two kinds of elements of O in the sample, and purity has reached 99.999%.Above result shows that the aluminum oxide for preparing has the characteristics such as purity is high, particle diameter is even.
Claims (4)
1. preparation method who is used for the high purity aluminium oxide of growing sapphire monocrystalline, it is characterized in that: High-Purity Aluminum Ammonium Sulfate is ground to obtain even-grained exsiccated ammonium alum precursor powder, then pyrolysis is carried out in its minute temperature section heating and removed by product, and obtain high-purity even-grained alumina powder jointed by further sintering.
2. the preparation method of the high purity aluminium oxide for the growing sapphire monocrystalline according to claim 1 is characterized in that:
A, take the High-Purity Aluminum Ammonium Sulfate crystal as raw material, raw material is fully ground, and places in the crucible;
B, raw material and crucible are done as a whole, placed in the process furnace, utilize self crystal water that reactant is dissolved at the 200-300 degree and dewater;
C, the reactant after will dewatering are heated to the 500-600 degree, remove ammonia;
D, reactant further is heated to the 850-950 degree, so that raw material decomposes fully, and sloughs SO in the raw material
3Deng by product;
E, at the 1000-1100 degree with the further sintering of product.
3. the preparation method of the high purity aluminium oxide for the growing sapphire monocrystalline according to claim 2, it is characterized in that: the process furnace that adopts is high temperature Muffle furnace.
4. the preparation method of the high purity aluminium oxide for the growing sapphire monocrystalline according to claim 1 and 2 is characterized in that: gaseous by-product one is connected with extraneous water straight through stainless steel tube in the whole reaction process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103720414A CN102863000A (en) | 2012-09-29 | 2012-09-29 | Preparation method of high-purity aluminum oxide for growth of sapphire monocrystalline |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103720414A CN102863000A (en) | 2012-09-29 | 2012-09-29 | Preparation method of high-purity aluminum oxide for growth of sapphire monocrystalline |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102863000A true CN102863000A (en) | 2013-01-09 |
Family
ID=47442178
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103720414A Pending CN102863000A (en) | 2012-09-29 | 2012-09-29 | Preparation method of high-purity aluminum oxide for growth of sapphire monocrystalline |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102863000A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104250017A (en) * | 2013-06-27 | 2014-12-31 | 山东沾化宝晶晶体科技有限公司 | Method for molding high-purity alumina for LED sapphire single crystal |
| CN112986250A (en) * | 2021-02-03 | 2021-06-18 | 大连理工大学 | Method for evaluating whether alkoxide method alumina meets growth requirement of colorless sapphire |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092382A (en) * | 1993-03-13 | 1994-09-21 | 山东淄博制酸厂 | High-purity ultra-fine alumina production technique and device |
| CN101327944A (en) * | 2008-07-16 | 2008-12-24 | 孙志昂 | Production process for preparing superfine crystal alpha-aluminum oxide by directly using aluminum sulfate |
-
2012
- 2012-09-29 CN CN2012103720414A patent/CN102863000A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092382A (en) * | 1993-03-13 | 1994-09-21 | 山东淄博制酸厂 | High-purity ultra-fine alumina production technique and device |
| CN101327944A (en) * | 2008-07-16 | 2008-12-24 | 孙志昂 | Production process for preparing superfine crystal alpha-aluminum oxide by directly using aluminum sulfate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104250017A (en) * | 2013-06-27 | 2014-12-31 | 山东沾化宝晶晶体科技有限公司 | Method for molding high-purity alumina for LED sapphire single crystal |
| CN104250017B (en) * | 2013-06-27 | 2016-01-13 | 山东沾化宝晶晶体科技有限公司 | The method that LED sapphire single-crystal high purity aluminium oxide is shaping |
| CN112986250A (en) * | 2021-02-03 | 2021-06-18 | 大连理工大学 | Method for evaluating whether alkoxide method alumina meets growth requirement of colorless sapphire |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103320899B (en) | Preparation method of nanometer aluminum nitride fiber | |
| Su et al. | Synthesis of kalsilite from microcline powder by an alkali-hydrothermal process | |
| CN102381723B (en) | Method for extracting aluminium oxide from pulverized fuel ash | |
| CN102826579A (en) | Preparation method of ultrahigh-purity and superfine aluminium oxide powder | |
| CN101880912B (en) | Aluminum hydroxide/magnesium-based hydrotalcite multiphase-based material and preparation method for crystal whiskers thereof | |
| WO2017080245A1 (en) | Method for preparing high-purity strontium hydroxide by using strontium slag | |
| CN103523810A (en) | Preparation method of high-purity aluminum oxide | |
| CN108658092B (en) | Method for preparing P-type molecular sieve and high-silicon mordenite from aluminum residue extracted by fly ash acid method and utilization method of fly ash | |
| CN102863000A (en) | Preparation method of high-purity aluminum oxide for growth of sapphire monocrystalline | |
| CN103121699B (en) | A kind of method that potassium fluosilicate prepares potassium fluoride | |
| CN104003428A (en) | Method for producing lithium hydroxide by dissolving spodumene out of pipeline reactor | |
| CN102275938A (en) | Method for preparing silicon dioxide nanotubes from halloysite used as raw material | |
| CN103738972A (en) | Method for preparing silicon micropowder by using pulverized fuel ash aluminum extraction residues | |
| CN102838141A (en) | Process for producing magnesium hydrate by removing silicon and aluminum from magnesite | |
| CN102491391A (en) | Preparation method for high-purity alumina | |
| Wang et al. | A clean method for gallium recovery and the coproduction of silica-potassium compound fertilizer and zeolite F from brown corundum fly ash | |
| CN1850624A (en) | Method for decomposing potash feldspar ore by low temperature wet process | |
| CN100363262C (en) | Method for producing alumina | |
| CN101195495A (en) | Process for producing high purity nano-lithium fluoride | |
| WO2014005498A1 (en) | Method for preparing aluminum dihydrogen tripolyphosphate | |
| CN102491392A (en) | Preparation method for aluminium oxide | |
| CN103214014B (en) | A kind of reaction unit and method thereof of producing aluminum oxide | |
| CN101654273A (en) | Production process for preparing aluminium fluoride by using ammonium bicarbonate | |
| CN103738989B (en) | A kind of middle-low bauxite produces the method for aluminum oxide | |
| CN102206865B (en) | Method for preparing mullite whisker from cyanite ore |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130109 |