CN103820107A - Method for removing carbon powder from fluorescent powder prepared by carbothermal reduction reaction - Google Patents
Method for removing carbon powder from fluorescent powder prepared by carbothermal reduction reaction Download PDFInfo
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- CN103820107A CN103820107A CN201410110969.4A CN201410110969A CN103820107A CN 103820107 A CN103820107 A CN 103820107A CN 201410110969 A CN201410110969 A CN 201410110969A CN 103820107 A CN103820107 A CN 103820107A
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Abstract
The invention relates to a method for removing carbon powder from fluorescent powder prepared by carbothermal reduction reaction. The method comprises the steps: (1) heating the fluorescent powder prepared by the carbothermal reduction reaction to the reaction temperature of 1,400-2,200K from room temperature in 5-200 minutes under nitrogen gas flow, carrying out heat preservation for 10-360 minutes, and then, slowly cooling to room temperature so that carbon powder and the fluorescent powder are separated from each other; and (2) removing the carbon powder, which serves as an outer-layer impurity phase, from the product obtained in the step (1). According to the method, a recrystallization-phase separation process, which is generated due to the difference between the temperature rise rate of the carbon powder and the temperature rise rate of the fluorescent powder during the temperature rise process, is utilize to achieve the effect of carbon removal; the participation of oxygen gas does not exist during carbon removal, so that the fluorescent powder is effectively prevented from oxidative deterioration, which is beneficial to the keeping of the quality of the fluorescent powder.
Description
Technical field
The present invention relates to a kind of method of utilizing phase disengagement method to remove remaining carbon dust in the fluorescent material that makes of carbothermic reduction, belong to materials chemistry field.
Background technology
The method that carbothermic reduction reaction is prepared fluorescent material is a kind of condition preparation method simple, with low cost, can greatly affect the luminescent properties of fluorescent material but obtain carbon dust remaining in product after reaction, and the application of this kind of method is limited greatly.At present the most general de-carbon method for to use combustion method de-carbon in oxygen, for example, discloses in Chinese patent CN101864311A in air ambient the high-temperature calcination of carbothermic reduction crude product has been removed to unnecessary carbon.But for the fluorescent material that utilizes carbothermic reduction reaction to make, this kind of method can allow fluorescent material deterioration by oxidation again in the time of heating, thereby cannot guarantee the maintenance of fluorescent material quality before and after de-carbon.
Summary of the invention
In the face of the problem that prior art exists, the object of the present invention is to provide a kind of phase disengagement method removal carbothermic reduction reaction that utilizes to make the method for remaining carbon dust in fluorescent material, thereby guarantee the maintenance of de-carbon front and back fluorescent material quality.
At this, the invention provides a kind of method of removing carbothermic reduction reaction and making carbon dust in fluorescent material, comprising:
(1) fluorescent material carbothermic reduction reaction being made rose to the temperature of reaction of 1400～2200K under stream of nitrogen gas in 5～200 minutes from room temperature, and slowly cooled to room temperature so that carbon dust wherein and fluorescent material are separated after being incubated 10～360 minutes; And the product of step (1) gained is removed the carbon dust as outer impurity phase by (2).
The present invention utilizes the recrystallization-phase separation of carbon dust and the different generations of fluorescent material temperature rise rate in temperature-rise period and then reaches the effect of de-carbon.De-carbon process does not have the participation of oxygen, effectively prevents fluorescent material deterioration by oxidation, is conducive to the maintenance of fluorescent material quality.And de-carbon process is carried out under reaction atmosphere and temperature of reaction, if therefore also have the raw material of complete reaction not in the carbothermic reduction reaction of preparing fluorescent material, in de-carbon process, can further react, thereby greatly improve the purity of fluorescent material.In addition, in the present invention the de-carbon time short, efficiently convenient, can obtain the fluorescent material that carbon content is extremely low.
In the present invention, treat that the fluorescent material that the described carbothermic reduction reaction of de-carbon makes can contain 0.05～30% carbon dust.Of the present invention applied widely, also can carry out de-carbon and obtain the fluorescent material that carbon content is extremely low up to 30% fluorescent material for carbon content.
Preferably, in step (1), described stream of nitrogen gas amount can be 0.01～1000mL/ minute.
Preferably, in step (1), the heating-up time is 10～60 minutes.
In the present invention, the carbon content of removing the fluorescent material after carbon dust can be 1～40% of the carbon content of the carbon dust before removing.The carbon content of removing the fluorescent material after carbon dust can be 0.02～0.5%.The present invention can obtain the extremely low fluorescent material of carbon content of purification by de-carbon process.
Preferably, the preparation of the fluorescent material that described carbothermic reduction reaction makes can comprise: take and contain the wherein raw material of each element by the stoichiometric ratio of described fluor, and add the carbon dust as reductive agent, ground and mixed is evenly powder raw material; And described powder raw material is carried out to carbothermic reduction reaction in specified temperature under reactant gases atmosphere make described fluorescent material.
Preferably, described reactant gases is the mixed gas of nitrogen and hydrogen.Preferably, in described reactant gases, the shared volume ratio of hydrogen is 0%～50%.
Preferably, described fluorescent material comprises silica-based nitride fluorescent material.
Accompanying drawing explanation
Fig. 1 is Sr before and after de-carbon
1.98si
5n
8: Eu
0.02the XRD figure picture of fluorescent material;
Fig. 2 is Sr before and after de-carbon
1.98si
5n
8: Eu
0.02the emmission spectrum of fluorescent material under 440nm optical excitation;
Fig. 3 is Sr before and after de-carbon
1.98si
5n
8: Eu
0.02the optical photograph of fluorescent material under natural light and UV-light, figure a is wherein the optical photograph under natural light before de-carbon, figure b is the optical photograph under natural light after de-carbon, and figure c is the optical photograph under UV-light before de-carbon, and figure d is the optical photograph under UV-light after de-carbon.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for the present invention is described, and unrestricted the present invention.
The invention provides and a kind ofly utilize phase disengagement method to remove carbothermic reduction reaction to make the method for remaining carbon dust in fluorescent material, utilize the recrystallization-phase separation of carbon dust and fluorescent material different generations of temperature rise rate in temperature-rise period and then reach the effect of de-carbon.
Preferably, the fluorescent material that carbothermic reduction reaction is made rises to the temperature (for example 1400～2200K) of regulation under shielding gas air-flow in 5～200 minutes (preferably 10～60 minutes) from room temperature, and slowly cools to room temperature after being incubated 10～360 minutes; Then the product of gained is removed to the carbon dust as outer impurity phase.Due in temperature-rise period, carbon dust is different from the temperature rise rate of fluorescent material, carbon dust is preferential to heat up to become and in heating, is formed centrally the reductive agent that the temperature difference serves as again simultaneously power is provided, the former pruinescence that causes carbon dust not to be reduced is around reduced to fluorescent material and assembles mutually with phase phosphor, the impurity that out-phase generates as carbon dust, reduction reaction etc. can only be present in the interface of fluorescent material phase, and final fluorescent material and impurity are separated.Like this, de-carbon process does not have the participation of oxygen, effectively prevents fluorescent material deterioration by oxidation, is conducive to the maintenance of fluorescent material quality.
More preferably, this shielding gas is nitrogen, and temperature of reaction when room temperature rises to carbothermic reduction reaction the process of preparing fluorescent material.Like this, nitrogen not only plays the effect of shielding gas, but also can be used as reactant gases.If therefore also contain in carbothermic reduction reaction the not raw material of complete reaction in this fluor, in de-carbon process, can further reaction under reaction atmosphere and temperature of reaction, thus greatly improve the purity of fluorescent material.
In one example, the fluorescent material that carbothermic reduction reaction can be made is put into heating unit (for example high frequency furnace), after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and in reaction process, continuing to pass into nitrogen assurance stream of nitrogen gas, airshed can be 0.01～1000mL/ minute.After nitrogen gas stream is stable, the temperature of reaction while the temperature of heating unit being risen in 5～200 minutes to carbothermic reduction reaction in the preparation process of fluorescent material, keeps this temperature to slowly cool to room temperature after 10～360 minutes.In addition, in order to obtain uniformed powder, can also grind.
The present invention, treats that the fluorescent material of de-carbon includes but not limited to silica-based nitride fluorescent material, for example, mix europium Sr
2si
5n
8, mix europium Ca
2si
5n
8, mix europium SrAlSiN
3deng.
In the present invention, the carbon containing fluorescent material of the fluorescent material for the treatment of de-carbon as long as making by carbothermic reduction reaction, and do not limit its concrete preparation process.In one example, carbothermic reduction is prepared fluorescent material and can be comprised the steps: to take and contain the wherein raw material of each element by the stoichiometric ratio of fluor, and adds the carbon dust as reductive agent, and ground and mixed is evenly powder raw material; And described powder raw material is carried out to carbothermic reduction reaction in specified temperature under reactant gases atmosphere make described fluorescent material.Wherein, grinding can be the grinding medium (for example alcohol and/or acetone) that adds 0.5～20 times of all raw material volume, in mortar, is ground to and mixes, and again, can be dried to obtain dry powder raw material after mixing.If raw material, because of dry and soft-agglomerated, can grind to form uniformed powder again in mortar.In addition, the reactant gases that carbothermic reduction reaction adopts can be the mixed gas of nitrogen and hydrogen, and wherein the shared volume ratio of hydrogen can be 0%～50%.Can adopt in one example throughput ratio is the N of 10:1
2/ H
2mixed gas.Temperature of reaction for example can be 1600K～2100K.
In addition, treat that the fluorescent material of de-carbon can also wash before heating, be dried, to remove in advance other impurity.For example can wash away salinity wherein for water, and reunite to prevent from drying process producing with absolute ethanol washing.
The raw material using in the present invention and chemical reagent can be analytical pure and above purity.
In the present invention, treat can contain 0.05～30% carbon dust in the fluorescent material of de-carbon.The carbon content of removing the fluorescent material after carbon dust can be the carbon dust before removal carbon content 1～40%.For example can obtain the uniformed powder of the carbon content 0.02～0.5% of purification.In addition, should be understood that in the present invention, can carry out repeatedly de-carbon process, with obtain carbon content still less, fluorescent material that purity is higher.
Fig. 1 illustrates de-carbon front and back Sr
1.98si
5n
8: Eu
0.02the XRD figure picture of fluorescent material, as shown in Figure 1, by de-carbon method of the present invention, in carbothermic reduction reaction not the raw material of complete reaction because further reaction generates target fluorescent material, thereby greatly improve the purity of fluorescent material.
Fig. 2 illustrates de-carbon front and back Sr
1.98si
5n
8: Eu
0.02the emmission spectrum of fluorescent material under 3440nm optical excitation, as shown in Figure 2, after de-carbon, because purity improves, luminous intensity strengthens fluorescent material, and 525nm place emission peak disappears, and utilizing emitted light purity increases.
Fig. 3 illustrates de-carbon front and back Sr
1.98si
5n
8: Eu
0.02the optical photograph of fluorescent material under natural light and UV-light, figure a is wherein the optical photograph under natural light before de-carbon, figure b is the optical photograph under natural light after de-carbon, figure c is the optical photograph under UV-light before de-carbon, figure d is the optical photograph under UV-light after de-carbon, as seen from Figure 3, fluorescent material body colour becomes utilizing emitted light under cleaning and ultraviolet lamp and becomes redness from yellow after de-carbon.
Method of the present invention is the continuity that carbothermic reduction reaction is prepared fluorescent material, there is carbothermic reduction reaction and prepare simple to operate, with low cost, the advantage such as output is large of fluorescent material, and also possess following advantage compared with the method for removing remaining carbon dust in the fluorescent material that carbothermic reduction makes with conventional combustion method:
1, de-carbon process does not have the participation of oxygen, effectively prevents fluorescent material deterioration by oxidation, is conducive to the maintenance of fluorescent material quality;
2, the de-carbon time is short, efficiently convenient;
If 3, also have the not raw material of complete reaction in carbothermic reduction reaction, in de-carbon process, can further react, greatly improve the purity of fluorescent material.
Further exemplify embodiment below to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter that following example is concrete etc. is only also an example in OK range, and those skilled in the art can be done in suitable scope and be selected by explanation herein, and do not really want to be defined in the below concrete numerical value of example.
Embodiment 1
(1) strontium oxide of Sr:Si:Eu:C=1.98:5:0.02:1 weighing in molar ratio, silicon nitride, europium sesquioxide, carbon dust are raw material, add alcohol or the acetone of 0.5 times of raw material volume to do grinding medium, in mortar, are ground to and mix;
(2) raw material mixing in step (1) being put into loft drier is dried
(3) by step (2) because dry and soft-agglomerated raw material grinds to form uniformed powder again in mortar;
(4) powder obtaining in step (3) is put into tube furnace and passed into reactant gases nitrogen and at the temperature of 1600K～2100K, react 10h with hydrogen (throughput ratio is 10:1), react complete and take out and make fluorescent material after body of heater is cooling;
(5) after dry the fluorescent material that contains carbon dust 0.05% washing obtaining in step (4), put into high frequency furnace, after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and in reaction process, continue to pass into nitrogen assurance stream of nitrogen gas;
(6) after nitrogen gas stream is stable, open high frequency furnace and temperature is risen in 10min to fluorescent material temperature of reaction in step (4), keep slowly cooling to room temperature after this temperature 30min-60min;
(7) product step (6) being obtained is removed outer impurity phase, grinds to form carbon content lower than 0.02% uniformed powder.Sr before and after de-carbon
1.98si
5n
8: Eu
0.02the XRD figure picture of fluorescent material, the emmission spectrum under 3440nm optical excitation, optical photograph under natural light and UV-light can be respectively referring to Fig. 1,2,3.As shown in Figure 1, through de-carbon process, the not SrSi of complete reaction
2o
2n
2further reaction is Sr
1.98si
5n
8: Eu
0.02thereby the purity of product is improved.As shown in Figure 2, Sr after de-carbon
1.98si
5n
8: Eu
0.02because purity improves, luminous intensity strengthens fluorescent material, and the emission peak at 525nm place disappears, and utilizing emitted light purity increases.As shown in Figure 3, fluorescent material body colour becomes utilizing emitted light under cleaning and ultraviolet lamp and becomes redness from yellow after de-carbon.
Embodiment 2
(1) calcium oxide of Ca:Si:Eu:C=1.98:5:0.02:8 weighing in molar ratio, silicon nitride, europium sesquioxide, carbon dust are raw material, add alcohol or the acetone of 1 times of raw material volume to do grinding medium, in mortar, are ground to and mix;
(2) raw material mixing in step (1) being put into loft drier is dried;
(3) by step (2) because dry and soft-agglomerated raw material grinds to form uniformed powder again in mortar;
(4) powder obtaining in step (3) is put into tube furnace and passed into reactant gases nitrogen and at the temperature of 1400K～2000K, react 10h with hydrogen (throughput ratio is 1:0), react complete and take out and make Ca after body of heater is cooling
1.98si
5n
8: Eu
0.02fluorescent material;
(5) by the Ca that contains carbon dust obtaining in step (4)
1.98si
5n
8: Eu
0.02after fluorescent material washing is dry, put into high frequency furnace, after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and in reaction process, continue to pass into nitrogen assurance stream of nitrogen gas;
(6) after nitrogen gas stream is stable, open high frequency furnace and temperature is risen in 10min to fluorescent material temperature of reaction in step (4), keep slowly cooling to room temperature after this temperature 100min;
(7) product step (6) being obtained is removed outer impurity phase, grinds to form the uniformed powder that carbon content is less than 0.5%.
Embodiment 3
(1) strontium oxide of Sr:Al:Si:Eu:C=0.98:1:1:0.02:3 weighing in molar ratio, aluminium nitride, silicon nitride, europium sesquioxide, carbon dust are raw material, add alcohol or the acetone of 1 times of raw material volume to do grinding medium, in mortar, are ground to and mix;
(2) raw material mixing in step (1) being put into loft drier is dried;
(3) by step (2) because dry and soft-agglomerated raw material grinds to form uniformed powder again in mortar;
(4) powder obtaining in step (3) is put into tube furnace and passed into reactant gases nitrogen and at the temperature of 1600K～2200K, react 10h with hydrogen (throughput ratio is 1:1), react complete and take out and make Sr after body of heater is cooling
0.98alSiN
3: Eu
0.02fluorescent material;
(5) by the Sr that contains carbon dust obtaining in step (4)
0.98alSiN
3: Eu
0.02after fluorescent material washing is dry, put into high frequency furnace, after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and in reaction process, continue to pass into nitrogen assurance stream of nitrogen gas;
(6) after nitrogen gas stream is stable, open high frequency furnace and temperature is risen in 10min to fluorescent material temperature of reaction in step (4), keep slowly cooling to room temperature after this temperature 60min;
(7) product step (6) being obtained is removed outer impurity phase, grinds to form uniformed powder.
Embodiment 4
(1) strontium oxide of Sr:Al:Si:Eu:C=0.98:1:1:0.02:3 weighing in molar ratio, aluminium nitride, silicon nitride, europium sesquioxide, carbon dust are raw material, add alcohol or the acetone of 10 times of raw material volumes to do grinding medium, in mortar, are ground to and mix;
(2) raw material mixing in step (1) being put into loft drier is dried;
(3) by step (2) because dry and soft-agglomerated raw material grinds to form uniformed powder again in mortar;
(4) powder obtaining in step (3) is put into tube furnace and passed into reactant gases nitrogen and at the temperature of 1600K～2200K, react 10h with hydrogen (throughput ratio is 2:1), react complete and take out and make Sr after body of heater is cooling
0.98alSiN
3: Eu
0.02fluorescent material;
(5) by the Sr that contains carbon dust obtaining in step (4)
0.98alSiN
3: Eu
0.02after fluorescent material washing is dry, put into high frequency furnace, after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and in reaction process, continue to pass into nitrogen assurance stream of nitrogen gas;
(6) after nitrogen gas stream is stable, open high frequency furnace and temperature is risen in 60min to fluorescent material temperature of reaction in step (4), keep slowly cooling to room temperature after this temperature 360min;
(7) product step (6) being obtained is removed outer impurity phase, grinds to form uniformed powder.
Embodiment 5
(1) calcium oxide of Ca:Si:Eu:C=1.98:5:0.02:5 weighing in molar ratio, silicon nitride, europium sesquioxide, carbon dust are raw material, add alcohol or the acetone of 3 times of raw material volumes to do grinding medium, in mortar, are ground to and mix;
(2) raw material mixing in step (1) being put into loft drier is dried;
(3) by step (2) because dry and soft-agglomerated raw material grinds to form uniformed powder again in mortar;
(4) powder obtaining in step (3) is put into tube furnace and passed into reactant gases nitrogen and at the temperature of 1400K～2000K, react 10h with hydrogen (throughput ratio is 5:1), react complete and take out and make Ca after body of heater is cooling
1.98si
5n
8: Eu
0.02fluorescent material;
(5) by the Ca that contains carbon dust obtaining in step (4)
1.98si
5n
8: Eu
0.02after fluorescent material washing is dry, put into high frequency furnace, after vacuumizing, pass into nitrogen to opening air outlet valve with outer normal atmosphere balance, and in reaction process, continue to pass into nitrogen assurance stream of nitrogen gas;
(6) after nitrogen gas stream is stable, open high frequency furnace and temperature is risen in 10min to fluorescent material temperature of reaction in step (4), keep slowly cooling to room temperature after this temperature 10min;
(7) product step (6) being obtained is removed outer impurity phase, grinds to form uniformed powder.
Industrial applicability: the present invention can remove carbon wherein in the situation that keeping fluorescent material quality, thereby greatly improves the purity of fluorescent material, and method of the present invention is simple, efficiently convenient, have great application prospect in fields such as white light LEDs.
Claims (9)
1. remove the method that carbothermic reduction reaction makes carbon dust in fluorescent material, it is characterized in that, comprising:
(1) fluorescent material carbothermic reduction reaction being made rose to the temperature of reaction of 1400～2200K under stream of nitrogen gas in 5～200 minutes from room temperature, and slowly cooled to room temperature so that carbon dust wherein and fluorescent material are separated after being incubated 10～360 minutes; And
(2) product of step (1) gained is removed to the carbon dust as outer impurity phase.
2. method according to claim 1, is characterized in that, in step (1), the fluorescent material that described carbothermic reduction reaction makes contains 0.05～30% carbon dust.
3. method according to claim 1 and 2, is characterized in that, in step (1), described stream of nitrogen gas amount is 0.01～1000mL/ minute.
4. according to the method in any one of claims 1 to 3, it is characterized in that, in step (1), the heating-up time is 10～60 minutes.
5. according to the method described in any one in claim 1 to 4, it is characterized in that, in step (2), the carbon content of removing the fluorescent material after carbon dust be the carbon dust before removing carbon content 1～40%.
6. according to the method described in any one in claim 1 to 5, it is characterized in that, the preparation of the fluorescent material that described carbothermic reduction reaction makes comprises: take and contain the wherein raw material of each element by the stoichiometric ratio of described fluor, and to add the carbon dust as reductive agent, ground and mixed be evenly powder raw material; And described powder raw material is carried out to carbothermic reduction reaction in specified temperature under reactant gases atmosphere make described fluorescent material.
7. method according to claim 6, is characterized in that, described reactant gases is the mixed gas of nitrogen and hydrogen.
8. method according to claim 7, is characterized in that, in described reactant gases, the shared volume ratio of hydrogen is 0%～50%.
9. according to the method described in any one in claim 1 to 8, it is characterized in that, described fluorescent material comprises silica-based nitride fluorescent material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104650861A (en) * | 2015-02-10 | 2015-05-27 | 江门市远大发光材料有限公司 | Simple method for preparing alkali-earth nitride red fluorescent powder |
| WO2018092696A1 (en) * | 2016-11-15 | 2018-05-24 | デンカ株式会社 | Red-emitting phosphor, light-emitting member, and light-emitting device |
| CN110577199A (en) * | 2018-06-07 | 2019-12-17 | 有研稀土新材料股份有限公司 | Method for removing carbon from nitride powder |
| CN111517804A (en) * | 2020-04-27 | 2020-08-11 | 中国科学院上海硅酸盐研究所 | Nitride red complex-phase fluorescent ceramic and preparation method thereof |
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| CN101117576A (en) * | 2006-07-31 | 2008-02-06 | 北京中村宇极科技有限公司 | Oxynitrides luminescent material and illuminating or exhibiting light source produced thereby |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104650861A (en) * | 2015-02-10 | 2015-05-27 | 江门市远大发光材料有限公司 | Simple method for preparing alkali-earth nitride red fluorescent powder |
| CN104650861B (en) * | 2015-02-10 | 2017-05-10 | 江门市远大发光材料有限公司 | Simple method for preparing alkali-earth nitride red fluorescent powder |
| WO2018092696A1 (en) * | 2016-11-15 | 2018-05-24 | デンカ株式会社 | Red-emitting phosphor, light-emitting member, and light-emitting device |
| CN110577199A (en) * | 2018-06-07 | 2019-12-17 | 有研稀土新材料股份有限公司 | Method for removing carbon from nitride powder |
| CN111517804A (en) * | 2020-04-27 | 2020-08-11 | 中国科学院上海硅酸盐研究所 | Nitride red complex-phase fluorescent ceramic and preparation method thereof |
| CN111517804B (en) * | 2020-04-27 | 2021-08-31 | 中国科学院上海硅酸盐研究所 | Nitride red complex-phase fluorescent ceramic and preparation method thereof |
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Application publication date: 20140528 |