CN1239671C - Method for producing superfine luminescent powder and equipment - Google Patents
Method for producing superfine luminescent powder and equipment Download PDFInfo
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- CN1239671C CN1239671C CN 200310100079 CN200310100079A CN1239671C CN 1239671 C CN1239671 C CN 1239671C CN 200310100079 CN200310100079 CN 200310100079 CN 200310100079 A CN200310100079 A CN 200310100079A CN 1239671 C CN1239671 C CN 1239671C
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Abstract
The present invention discloses a method for manufacturing ultrathin fluorescent powder (luminescent materials) by spray combustion and production equipment for using the method. The method comprises the following steps: (1) preparing metal soluble salt solutions; (2) preparing non-metallic compound solutions, and adding the non-metallic compound solutions in the metal soluble salt solutions so as to obtain mixed solutions; (3) adding incendiary agents and additives in the mixed solution so as to form feed liquid; (4) sufficiently atomizing the feed liquid, and carrying out combustion reaction with hot air so as to obtain precursors of fluorescent powder; (5) calcining the precursors under the condition of a certain atmosphere so as to obtain powder bodies of ultrathin fluorescent powder. By using the method and the equipment, the ultrathin fluorescent powder of which the medium particle diameter is in a scope from 2 to 5 mu m can be manufactured. Obtained fluorescent powder has the advantages of favorable luminous performance and painting performance, and the method has the advantages of high luminous efficiency of corresponding equipment, energy saving, environmental protection and continuous production.
Description
Technical field
Originally relate to manufacture method and equipment thereof that invention relates to a kind of superfine fluorescent powder.
Background technology
Combustion method is a kind ofly to cause at a certain temperature by presoma, by the carrying out that the burning liberated heat of incendiary material is kept reaction, makes the method for ceramic powder rapidly.Have resultant velocity fast (being reflected at 5-10 finished in the time of second), the product granularity is little, and pattern is controlled, the product purity height, and advantage such as energy-conservation is a focus of Recent study.Since the eighties of last century the nineties, how tame research institution begins combustion method is applied to the preparation of fluorescent material both at home and abroad, particularly is used for preparing nano-phosphor, causes the industry common concern.But, make a general survey of present Patent document data, wherein related mainly is the preparation of fluorescent material in a small amount, the Processes and apparatus of none suitability for industrialized production, and major part all is to utilize the crucible feed liquid of packing into, place under 500-800 ℃ the temperature and finish reaction, because product is fluffy unusually, therefore the crucible one of 800ml is produced product only less than 50 grams, production efficiency is very low, not only do not bring into play the fast advantage of its resultant velocity, and serious waste electric energy and heat energy, very big practical value not.In addition, aforesaid method can't be handled the waste gas that can produce in the incendiary material combustion processes, cause environmental pollution easily.
Summary of the invention
The purpose of this invention is to provide a kind of manufacture method that makes the superfine fluorescent powder that luminescent properties is good, particle size is controlled in 2nm-5 μ m, granule-morphology is controlled, coating property is good, is a kind of method of making superfine fluorescent powder by spray burning.
Another object of the present invention provides a kind of by the employed equipment of spray burning manufacturing superfine fluorescent powder.
For achieving the above object, the present invention takes following technical scheme:
A kind of method by spray burning manufacturing superfine fluorescent powder, this method comprises the steps:
(1), according to the weight of the target fluorescent material that will make, convert and take by weighing the weight of the water soluble salt of target fluorescent material institute metal ion according to stoichiometric ratio, be dissolved in water respectively, stir, the pH value of regulator solution obtains metal salt solution to 5.5-8.5;
(2), according to the weight of the target fluorescent material that will make, convert and take by weighing the weight of the water soluble compound of the contained non-metallic element of target fluorescent material according to stoichiometric ratio, be dissolved in water respectively, add in the metal salt solution that obtains in the step (1), obtain mixing solutions:
(3), according to the weight of the target fluorescent material that will make, take by weighing incendiary material and additive according to the incendiary material of the required cooperation of manufacturing objective fluorescent material and the weight of additive, add obtaining in the mixing solutions in the step (2), form feed liquid;
(4), the feed liquid that obtains in the step (3) is added in the spraying gun, fully atomizing, from spraying gun, spray, the drop of ejection contacts with the air of heat, combustion reactions takes place, and utilizes the powder collector to collect from the resulting powder of discharge port washing, obtain the fluorescent material presoma, and discharge gas at relief outlet;
(5), with the fluorescent material presoma that obtains in the step (4) crucible of packing into, place High Temperature Furnaces Heating Apparatus, carry out high-temperature calcination according to target fluorescent material desired atmosphere, temperature in high-temperature calcination, come out of the stove, pulverize, grind, obtain the powder of superfine fluorescent powder.
Make in the method for superfine fluorescent powder in the above-mentioned spray burning of passing through, also comprise step (6): the powder that obtains in the step (5) is carried out surface treatment.
Make in the method for superfine fluorescent powder in the above-mentioned spray burning of passing through, described method also comprises step (5) ': expellant gas in the step (4) is adopted back-off hydraucone formula ventilating mode, feed in the vent gas treatment agent and carry out vent gas treatment, wherein, the vent gas treatment agent contains at least a in the ammonia soln of the NaOH aqueous solution of aqueous nitric acid, 0.15wt% of aqueous hydrochloric acid that concentration is 0.15wt%, 0.1-5wt% and 0.1-10wt%.
Pass through spray burning and make in the method for superfine fluorescent powder above-mentioned, described target fluorescent material is that CRT, PDP, FED, FID, EL etc. show any with in the used fluorescent material of illuminating device such as fluorescent material and LED, electricity-saving lamp, luminescent lamp, high voltage mercury lamp, metal halide lamp.
Pass through spray burning and make in the method for superfine fluorescent powder above-mentioned, in described step (1), the water soluble salt of described target fluorescent material institute metal ion is a nitrate, one or more in hydrochloride (muriate) and the vitriol.
Make in the method for superfine fluorescent powder in the above-mentioned spray burning of passing through, in described step (3), described incendiary material is urea (urea), glycine (Padil), citric acid (2-hydroxyl-1, at least a in the water-soluble organic compounds such as EDTA acid (ethylenediamine tetraacetic acid (EDTA)) 2,3-tricarballylic acid),, EDTA two ammoniums (ethylenediamine tetraacetic acid (EDTA) ammonium) and thiocarbamide.
Make in the method for superfine fluorescent powder in the above-mentioned spray burning of passing through, in described step (3), the weight of described incendiary material is the 0.2wt%-500wt% of target fluorescent material weight, looks different target fluorescent material and required particle size thereof, pattern and the ratio of regulating incendiary material.
Pass through spray burning and make in the method for superfine fluorescent powder above-mentioned, in described step (5), the number of times of described high-temperature calcination is at least once.
Pass through spray burning and make in the method for superfine fluorescent powder above-mentioned, in described step (5), the atmosphere of described high-temperature calcination is at least a in air, nitrogen, hydrogen and the CO gas.
Make in the method for superfine fluorescent powder in the above-mentioned spray burning of passing through, in described step (4), described washing process is the difference according to target fluorescent material, select content be the aqueous hydrochloric acid of x, aqueous nitric acid that content is x and content be x NaOH solution in a kind of, wherein, 0wt%＜x≤5wt% washs 3-5 time, is washed till neutrality with deionized water then.
Make in the method for superfine fluorescent powder in the above-mentioned spray burning of passing through, in described step (4), the temperature of the air of described heat is 250-800 ℃.
A kind of used equipment of method of making superfine fluorescent powder by spray burning, this equipment includes High Temperature Furnaces Heating Apparatus, washing device, it is characterized in that: this equipment also includes the spray burning device, this spray burning device is to adopt the reservoir that is provided with agitator, its outlet is by the liquid-inlet in the liquid-transport pipe-line connection spraying gun, and is furnished with airheater, its hot air outlet connects the gas feed of spraying gun by gas pipe line, under spraying gun, be provided with the spray burning chamber, and the outlet of spraying gun is stretched in the spray burning chamber, and the outlet in spray burning chamber connects the import of product collector.
In above-mentioned equipment, the import of described airheater connects air filter, gas blower or air compressor by gas pipe line.
In above-mentioned equipment, the outlet of the tail gas of described product collector connects exhaust gas treating device by gas pipe line, induced draft fan.
In above-mentioned equipment, the liquid-transport pipe-line between described reservoir and the spraying gun is provided with feed liquid strainer, dehvery pump.
In above-mentioned equipment, described High Temperature Furnaces Heating Apparatus is a kind of in chamber type electric resistance furnace, tunnel like resistance furnace and the rotary type resistance furnace.
In above-mentioned equipment, described spraying gun is a kind of in rotary atomizer (utilizing centrifugal energy), air flow type jet nozzle, pressure nozzle and the acoustic energy spraying gun.
In above-mentioned equipment, described product collector is at least a in cyclonic separator, wet cleaner, electrostatic precipitator and the cloth envelop collector, the product collector is a product collector of employing flash trapping stage mode, or for adopting a plurality of product collectors of the isolating collection mode of plural serial stage.
In equipment of the present invention, employed spraying gun, product collector, High Temperature Furnaces Heating Apparatus are known equipment.
Advantage of the present invention is:
Method of the present invention is by feed liquid is atomized back and pyritous air streams contact, finish burning, i.e. so-called " spray burning method ", preparation fluorescent material presoma, presoma is carried out high-temperature calcination under certain atmosphere, carry out surface treatment at last and can make the luminescent material that luminescent properties is good, particle size is controlled in 2nm-5 μ m, granule-morphology is controlled, coating property is good, luminescent properties is good.This method can prepare CRT, PDP, FED, FID etc. and show that the use of this fluorescent material can improve the luminous efficiency of relevant device with illuminating device fluorescent material such as fluorescent material and LED, electricity-saving lamp, luminescent lamp, high voltage mercury lamp, metal halide lamps.Equipment of the present invention has the tail gas clean-up retrieving arrangement, avoids in the incendiary material combustion processes the direct discharging of the waste gas that can produce, and has saved electric energy and heat energy, is a kind of energy-saving and environmental protection, preparation method efficiently, is fit to continuous production.
Description of drawings
Fig. 1 is the preparation flow synoptic diagram of the method for spray burning manufactured superfine fluorescent powder
Fig. 2 uses the atomized firing equipment synoptic diagram for the method for spray burning manufactured superfine fluorescent powder
Fig. 3 uses the exhaust gas treating device synoptic diagram of atomized firing equipment for the method for spray burning manufactured superfine fluorescent powder
Fig. 4 uses the powder collecting device synoptic diagram of atomized firing equipment for the method for spray burning manufactured superfine fluorescent powder
Fig. 5 is ultra-fine (Y, Gd) BO that utilizes the spray burning manufactured
3: the emmission spectrum of Eu fluorescent material (excitaton source: wavelength is the VUV of 147nm)
Fig. 6 is ultra-fine (Y, Gd) BO that utilizes the spray burning manufactured
3: the SEM photo of Eu fluorescent material, adopt JSM-840 electron microscope to take
Embodiment
The preparation flow synoptic diagram of the method by spray burning manufactured superfine fluorescent powder of the present invention as shown in Figure 1, in step (1), the preparing metal soluble salt solution; In step (2), preparation nonmetallic compound solution, and, obtain mixing solutions with in the metal soluble salt solution that obtains in this nonmetallic compound solution adding step (1); In step (3), with incendiary material and additive, add obtaining in the mixing solutions in the step (2), form feed liquid; In step (4), the feed liquid that obtains in the step (3) is fully atomized, and with warm air generation combustion reactions, obtain the fluorescent material presoma; In step (5), the fluorescent material presoma that obtains in the step (4) is calcined under certain atmosphere, obtain the powder of superfine fluorescent powder; In step (6), the powder that obtains in the step (5) is carried out surface treatment, obtain final product-superfine fluorescent powder.
Institute's use equipment of the method by spray burning manufactured superfine fluorescent powder of the present invention, as shown in Figure 2, this equipment is to adopt reservoir 1, be provided with agitator in it, the outlet at bottom of reservoir 1 connects feed liquid strainer 2 successively by liquid-transport pipe-line 14, dehvery pump 3, connect the liquid-inlet in the spraying gun 4, air filter 7 is by gas pipe line 15, connect gas blower or air compressor 8 successively, airheater 6, connect the gas feed of spraying gun 4, be provided with spray burning chamber 9 under spraying gun 4, the jet hole of spray outlet 5 stretches in spray burning chamber 9, two outlets in the bottom in spray burning chamber 9 product collector 10 of practicing midwifery respectively, secondary product collector 11.The tail gas outlet of product collector 10, secondary product collector 11 connects exhaust gas treating device 13 by gas pipe line 15, induced draft fan 12.
Exhaust gas treating device as shown in Figure 3, exhaust gas treating device 13 is to be a container, feed gas pipe line 15 in it, the port that feeds gas pipe line 15 in the exhaust gas treating device 13 connects back-off hydraucone 16, in these back-off hydraucone 16 straight-through vent gas treatment agent 17, but be provided with the tail gas that relief outlet 18 emission treatment are crossed on the top of exhaust gas treating device 13, or connect vent pipe feeding second cleaner (being the secondary exhaust gas treating device).By the isolated tail gas of product collector through gas pipe line 15, enter in the exhaust gas treating device 13, and by in the straight-through vent gas treatment agent 17 of back-off hydraucone 16, carry out vent gas treatment after, the tail gas of handling feeds second cleaners (being the secondary exhaust gas treating device) or direct the discharging through relief outlet 18.
As shown in Figure 4, the product collector can be made up of solid and gas separator 19 and container 20.Carry reaction product secretly from the discharge port effluent stream in spray burning chamber 9 and enter solid and gas separator 19, after the separation by solid and gas separator 19, the powder of superfine fluorescent powder falls into container 20, and tail gas is by induced draft fan 12, through gas pipe line 15, enter in the exhaust gas treating device 13.
The concrete implementation process of the present invention is:
Take by weighing the water soluble salt of a certain amount of target fluorescent material institute metal ion according to stoichiometric ratio, be dissolved in water respectively, stir, to the 6-8, obtain metal salt solution with the pH value of a kind of regulator solution in ammoniacal liquor, the NaOH aqueous solution, aqueous hydrochloric acid and the aqueous nitric acid.As shown in Figure 2, take by weighing the water soluble compound of the contained non-metallic element of a certain amount of fluorescent material, be dissolved in water respectively, add in the metal salt solution, obtain mixing solutions and add in the reservoir 1 and stir according to stoichiometric ratio.Take by weighing a certain proportion of incendiary material and additive then, add reservoir 1, stir 5 minutes, obtain feed liquid by 1 hour.Utilize dehvery pump 3 to add in the spraying gun 4 feed liquid, ejection from spray outlet 5, fully atomizing by liquor charging pipeline 14.Open airheater 6 and gas blower or air compressor 8, the formation air communication is crossed airheater 6 and is heated, and Heating temperature is 250-800 ℃.The drop of ejection contacts with the air of heat from spray outlet 5, in spray burning chamber 9 combustion reactions takes place, because drop is less, finishes but react moment.Air-flow is carried reaction product secretly and is flowed out from discharge port.Collect resulting powder by product collector 10, the tail gas behind the collection powder enters exhaust gas treating device 13 by gas pipe line 15.The part powder enters secondary product collector 11 to be separated, and collects, and the tail gas behind the collection powder enters exhaust gas treating device 13 by gas pipe line 15.The powder that washing obtains obtains the fluorescent material presoma.With the fluorescent material presoma crucible of packing into, place High Temperature Furnaces Heating Apparatus, in certain atmosphere, carry out high-temperature calcination, come out of the stove, pulverize, grind.The powder that obtains is carried out surface treatment, obtain superfine fluorescent powder of the present invention.
Actual implementation process of the present invention and to be not limited to above details described, wherein part steps can be deleted with the composition and the requirement of realistic objective fluorescent material.
Embodiment
Spray burning manufactured 2000g ultra-fine (Y, Gd) BO
3: Eu fluorescent material.
Take by weighing corresponding rare-earth oxide according to stoichiometric ratio, use nitric acid dissolve respectively, thin up adds reservoir to 0.4mol/l, regulates pH value to 6.5 with the ammoniacal liquor of 5wt%.Take by weighing H according to stoichiometric ratio
3BO
3, be made into the aqueous solution of 1mol/l, add reservoir, take by weighing glycine 500g, be dissolved in water, add reservoir, add 10gNa
2SO
4..Stirred 5 minutes.Utilize dehvery pump to pass through liquor charging pipeline 14 feed liquid and add in equipment 2 spraying guns shown in Figure 2, ejection, fully atomizing from pressure nozzle 5 (spraying gun adopts pressure nozzle the present embodiment).Open airheater 6 shown in Figure 2 and gas blower 8 and form air communication and cross airheater 6 and heat, being heated to gas flow temperature is 550 ℃.The drop of ejection contacts with the air of heat from pressure nozzle 5, in spray burning chamber 9 combustion reactions takes place.Air-flow is carried reaction product secretly and is flowed out from discharge port.Collect the resulting powder of 10 (the product collector is to adopt electrostatic dust collection equipment 10 in the present embodiment) by electrostatic dust collection equipment, tail gas behind the collection powder enters exhaust gas treating device 13 by gas pipe line 15, vent gas treatment liquid one-level adopts the aqueous hydrochloric acid of 5wt%, and secondary adopts the NaOH aqueous solution of 5wt%.The powder that washing obtains obtains the fluorescent material presoma.With the fluorescent material presoma crucible of packing into, place High Temperature Furnaces Heating Apparatus, in air atmosphere, 1000 ℃ were carried out high-temperature calcination 1 hour, came out of the stove, and pulverized, and ground.The powder that obtains is scattered in 100ml, and concentration is the Y (NO of 0.1mol/l
3)
3In the aqueous solution, the ammoniacal liquor that stirs and drip concentration rapidly and be 0.1mol/l precipitates, and filters the turbid liquid of gained, and with deionized water wash 2 times, with raw spirit washing 2 times, oven dry obtains ultra-fine (Y, Gd) BO
3: Eu fluorescent material.
The luminescent spectrum of embodiment as shown in Figure 5.The SEM photo of embodiment is (JSM-840electron microscope) as shown in Figure 6.The spectrum that Fig. 5 shows is compared with the luminescent material of the same type of general commercial has higher luminous intensity, purity of color preferably.And Fig. 6 shows that the particle size of this luminescent material is about 80nm, and has pattern preferably.
Claims (18)
1, a kind of method by spray burning manufacturing superfine fluorescent powder, it is characterized in that: this method comprises the steps:
(1), according to the weight of the target fluorescent material that will make, convert and take by weighing the weight of the water soluble salt of target fluorescent material institute metal ion according to stoichiometric ratio, be dissolved in water respectively, stir, the pH value of regulator solution obtains metal salt solution to 5.5-8.5;
(2), according to the weight of the target fluorescent material that will make, convert and take by weighing the weight of the water soluble compound of the contained non-metallic element of target fluorescent material according to stoichiometric ratio, be dissolved in water respectively, add in the metal salt solution that obtains in the step (1), obtain mixing solutions;
(3), according to the weight of the target fluorescent material that will make, take by weighing incendiary material and additive according to the incendiary material of the required cooperation of manufacturing objective fluorescent material and the weight of additive, add obtaining in the mixing solutions in the step (2), form feed liquid;
(4), the feed liquid that obtains in the step (3) is added in the spraying gun, fully atomizing, from spraying gun, spray, the drop of ejection contacts with the air of heat, combustion reactions takes place, and utilizes the powder collector to collect from the resulting powder of discharge port washing, obtain the fluorescent material presoma, and discharge gas at relief outlet;
(5), with the fluorescent material presoma that obtains in the step (4) crucible of packing into, place High Temperature Furnaces Heating Apparatus, carry out high-temperature calcination according to target fluorescent material desired atmosphere, temperature in high-temperature calcination, come out of the stove, pulverize, grind, obtain the powder of superfine fluorescent powder.
2, the method by spray burning manufacturing superfine fluorescent powder according to claim 1, it is characterized in that: described method also comprises step (6): the powder that obtains in the step (5) is carried out surface treatment.
3, the method for making superfine fluorescent powder by spray burning according to claim 1 and 2, it is characterized in that: described method also comprises step (5) ': expellant gas in the step (4) is adopted back-off hydraucone formula ventilating mode, feed in the vent gas treatment agent and carry out vent gas treatment, wherein, the vent gas treatment agent contains at least a in the ammonia soln of the NaOH aqueous solution of aqueous nitric acid, 0.1-5wt% of aqueous hydrochloric acid that concentration is 0.1-5wt%, 0.1-5wt% and 0.1-10wt%.
4, according to claim 1 and 2ly make the method for superfine fluorescent powder by spray burning, it is characterized in that: described target fluorescent material is that CRT, PDP, FED, FID, EL show any with in fluorescent material and LED, electricity-saving lamp, luminescent lamp, high voltage mercury lamp, the used fluorescent material of metal halide lamp illuminating device.
5, the method for making superfine fluorescent powder by spray burning according to claim 1 and 2, it is characterized in that: in described step (1), the water soluble salt of described target fluorescent material institute metal ion is a nitrate, one or more in hydrochloride and the vitriol.
6, the method for making superfine fluorescent powder by spray burning according to claim 1 and 2, it is characterized in that: in described step (3), described incendiary material is at least a in the water-soluble organic compounds of urea, glycine, citric acid, ethylenediamine tetraacetic acid (EDTA), ethylenediamine tetraacetic acid (EDTA) ammonium and thiocarbamide.
7, the method for making superfine fluorescent powder by spray burning according to claim 6, it is characterized in that: in described step (3), the weight of described incendiary material is the 0.2wt%-500wt% of target fluorescent material weight, looks different target fluorescent material and required particle size thereof, pattern and the ratio of regulating incendiary material.
8, according to claim 1 and 2ly make the method for superfine fluorescent powder by spray burning, it is characterized in that: in described step (5), the number of times of described high-temperature calcination is at least once.
9, according to claim 1 and 2ly make the method for superfine fluorescent powder by spray burning, it is characterized in that: in described step (5), the atmosphere of described high-temperature calcination is at least a in air, nitrogen, hydrogen and the CO gas.
10, the method for making superfine fluorescent powder by spray burning according to claim 1 and 2, it is characterized in that: in described step (4), described washing process is the difference according to target fluorescent material, select content be the aqueous hydrochloric acid of x, aqueous nitric acid that content is x and content be x NaOH solution in a kind of, wherein, 0wt%＜x≤5wt% washs 3-5 time, is washed till neutrality with deionized water then.
11, the method by spray burning manufacturing superfine fluorescent powder according to claim 1 and 2, it is characterized in that: in described step (4), the temperature of the air of described heat is 250-800 ℃.
12, the described used equipment of method of making superfine fluorescent powder by spray burning of a kind of claim 1, this equipment includes High Temperature Furnaces Heating Apparatus, washing device, it is characterized in that: this equipment also includes the spray burning device, this spray burning device is to adopt the reservoir that is provided with agitator, its outlet is by the liquid-inlet in the liquid-transport pipe-line connection spraying gun, and is furnished with airheater, its hot air outlet connects the gas feed of spraying gun by gas pipe line, under spraying gun, be provided with the spray burning chamber, and the outlet of spraying gun is stretched in the spray burning chamber, and the outlet in spray burning chamber connects the import of product collector.
13, equipment according to claim 12 is characterized in that: the import of described airheater connects air filter, gas blower or air compressor by gas pipe line.
14, according to claim 12 or 13 described equipment, it is characterized in that: the tail gas outlet of described product collector connects exhaust gas treating device by gas pipe line, induced draft fan.
15, according to claim 12 or 13 described equipment, it is characterized in that: the liquid-transport pipe-line between described reservoir and the spraying gun is provided with feed liquid strainer, dehvery pump.
16, according to claim 12 or 13 described equipment, it is characterized in that: described High Temperature Furnaces Heating Apparatus is a kind of in chamber type electric resistance furnace, tunnel like resistance furnace and the rotary type resistance furnace.
17, according to claim 12 or 13 described equipment, it is characterized in that: described spraying gun is a kind of in rotary atomizer, air flow type jet nozzle, pressure nozzle and the acoustic energy spraying gun.
18, according to claim 12 or 13 described equipment, it is characterized in that: described product collector is at least a in cyclonic separator, wet cleaner, electrostatic precipitator and the cloth envelop collector, the product collector is a product collector of employing flash trapping stage mode, or for adopting a plurality of product collectors of the isolating collection mode of plural serial stage.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310100079 CN1239671C (en) | 2003-10-09 | 2003-10-09 | Method for producing superfine luminescent powder and equipment |
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|---|---|---|---|
| CN 200310100079 CN1239671C (en) | 2003-10-09 | 2003-10-09 | Method for producing superfine luminescent powder and equipment |
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| CN1239671C true CN1239671C (en) | 2006-02-01 |
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| CN103386284A (en) * | 2012-05-11 | 2013-11-13 | 四川汇利实业有限公司 | Production system for pharmaceutical workshop |
| CN102810666B (en) * | 2012-08-01 | 2014-10-22 | 四川大学 | Preparation method of anode material LiMxNiyMn2-x-yO4 |
| CN113830816A (en) * | 2021-04-28 | 2021-12-24 | 广东石油化工学院 | Process for synthesizing multi-metal nano oxide by using confined combustion effect in high-dispersion hot spot |
| CN113262737A (en) * | 2021-06-17 | 2021-08-17 | 江阴讯安新材料科技有限公司 | Laser-induced synthesis equipment and synthesis method of nano bismuth oxide |
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