CN110499154A - A kind of preparation method of Bi doping borofluoride - Google Patents
A kind of preparation method of Bi doping borofluoride Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of Bi doping borofluoride, are related to luminescent material technical field, and preparation method is the following steps are included: (1) is pre-sintered: weighing SrCO3、SrF2、H3BO3、Bi2O3Grinding, moves in crucible, is pre-sintered in high-temperature calcination stove, and pre-sintering temperature is 500-800 DEG C, time 3-7h；(2) preparation of fluorescent powder: after being cooled to room temperature, grinding is sintered 5-8h, cooled to room temperature is sintered 5-8h at 800-1400 DEG C again at 800-1400 DEG C after mixing；Cooled to room temperature, grinding, can obtain Sr5(BO3)3F:x%Bi, wherein 0.01≤x≤15.The present invention synthesizes various concentration Bi by using high temperature solid-state method in air3+The Sr of doping5(BO3)3The bluish-green emitting phosphor of F:x%Bi, light-emitting phosphor is high-efficient, and luminescent properties enhancing, physicochemical properties are stablized, and preparation process environmental protection, preparation cost is low, easy to operate.
Description
Technical field
The present invention relates to luminescent material technical fields, and in particular to a kind of preparation method of Bi doping borofluoride.
Background technique
Bismuth (Bi) element causes the electron configuration of bismuth ion to be easy to lose electricity since outer shell electronics is not completely filled
Therefore son there are the bismuth ion of a variety of valence states and is easily formed cluster in compound.Due to the exposed electricity of bismuth ion outermost layer
Sub- configuration, shining for bismuth ion is very sensitive to the variation of crystalline environment field around it, such as: when the dopant material for changing bismuth ion
Matrix, regulate and control field environment around bismuth ion, can make bismuth ion shine from ultraviolet light change to blue and green light even to
Yellow light forms the very wide fluorescence spectrum of transmitting range.
The bismuth ion of positive trivalent is most common and most stable of bismuth ion valence state in nature.The Bi in different substrates3+From
The fluorescent characteristic of son is by systematic research.In general, Bi3+The photon of Ions Absorption ultra-violet (UV) band, launches from 300nm to 650nm
Blue green light broad emission band.Bi3+The material of ion doping also has excellent performance in white light LEDs field, in white light LED fluorescent powder
In, Bi3+Ion is commonly used to absorb black light and transfer energy to shining in green wavelength.And bismuth is a kind of nontoxic
Harmless environment protection metal, referred to as " green bismuth ".Importantly, the cost of bismuth is low, it is unique nontoxic trivalent heavy metals ion,
Many fields have great attraction, and its property is similar in some aspects to rare earth ion, so if with bismuth from
Cost can not only be reduced when rare earth ion, in this way application in son substitution matrix but also can be reduced pollution to environment and
Harm to organism.
At present due to lack efficient stable blue-green fluorescent powder, LED shine there are colour renderings it is poor, colour temperature is high the problems such as.
Most popular blue-green fluorescent powder physicochemical property is unstable currently on the market, and not environmentally, preparation cost is high by preparation process, uses
The pollution of heavy metal or nitride to environment and the harm to organism.Although having been used for commercial object, show
It is not able to satisfy the demand of people so.
In pervious report, although there are much discussion about boric acid system, it is based on Sr5(BO3)3The fluorescent powder of F
Seldom it is discussed.There is presently no about based on Sr5(BO3)3The Bi of F3+The research report of doping fluorescent powder.
Summary of the invention
In order to overcome the deficiencies of the prior art, the present invention passes through in providing a kind of preparation method of Bi doping borofluoride
Using high temperature solid-state method, various concentration Bi is synthesized in air3+The Sr of doping5(BO3)3The bluish-green emitting phosphor of F:x%Bi, it is glimmering
Light powder luminous efficiency is high, and luminescent properties enhancing, physicochemical properties are stablized, and preparation process environmental protection, preparation cost is low, operation letter
Just.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of preparation method of Bi doping borofluoride, comprising the following steps:
(1) it is pre-sintered: weighing SrCO respectively by raw material proportioning3、SrF2、H3BO3、Bi2O3It is ground in agate mortar, then will
Mixed powder moves in crucible, and is put into high-temperature calcination stove and is pre-sintered, and pre-sintering temperature is 500-800 DEG C, pre-burning
The knot time is 3-7h；
(2) after agglutinating matter obtained by handling through step (1) is cooled to room temperature, gains the preparation of fluorescent powder: are taken out
It is placed again into agate mortar and grinds, be sintered 5-8h at 800-1400 DEG C after mixing, cooled to room temperature exists again
5-8h is sintered at 800-1400 DEG C；Gains cooled to room temperature, and it is ground to powder, Bi doping borofluoride can be obtained
Sr5(BO3)3F:x%Bi, wherein 0.01≤x≤15.
Preferably, 0.5≤x≤10.It is further preferred that 1≤x≤7.
Preferably, when 1≤x≤3, in the step (2), sintering temperature is 800-1100 DEG C, sintering time 7-8h, from
It is so cooled to room temperature, is sintered 7-8h at 800-1100 DEG C again；When 3≤x≤7, in the step (2), sintering temperature is
1100-1400 DEG C, time 5-7h, cooled to room temperature is sintered 5-7h at 1100-1400 DEG C again.
Preferably, it in the step (1), is ground 10-40 minutes in agate mortar.
Preferably, in the step (2), taking-up gains, which are placed again into agate mortar, to be ground 5-20 minutes.
Compared with prior art, the present invention has the following advantages and beneficial effects:
The present invention uses high temperature solid-state method, synthesizes various concentration Bi in air3+The Sr of doping5(BO3)3F:x%Bi is glimmering
Light powder, by adulterating trivalent Bi ion, produces this material using fluoboric acid strontium as the novel energy-saving environment-friendly luminescent material of matrix
Raw broadband blue green light, broadband blue green light adjustability is very strong, has good potential application adjusting LED white light.The base of this material
Matter fluoboric acid strontium and the major element Bi toxicity of doping are low, and price is also cheap many relative to rare earth, and luminous efficiency is obvious
Height, luminescent properties enhancing, physicochemical properties are stablized, and preparation cost is low, easy to operate.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is Sr in embodiment5(BO3)3The XRD spectrum of F:1%Bi fluorescent powder.
Fig. 2 is Sr in embodiment5(BO3)3The XRD spectrum of F:3%Bi fluorescent powder.
Fig. 3 is Sr in embodiment5(BO3)3The XRD spectrum of F:5%Bi fluorescent powder.
Fig. 4 is Sr in embodiment5(BO3)3The XRD spectrum of F:7%Bi fluorescent powder.
Fig. 5 is Sr in embodiment5(BO3)3Fluorescence spectrum of the F:1%Bi fluorescent powder in the case where fluorescence emission wavelengths are 315nm
Figure.
Fig. 6 is Sr in embodiment5(BO3)3Fluorescence spectrum of the F:1%Bi fluorescent powder in the case where fluorescence exciting wavelength is 526nm
Figure.
Fig. 7 is Sr in embodiment5(BO3)3Fluorescence spectrum of the F:3%Bi fluorescent powder in the case where fluorescence emission wavelengths are 315nm
Figure.
Fig. 8 is Sr in embodiment5(BO3)3Fluorescence spectrum of the F:3%Bi fluorescent powder in the case where fluorescence exciting wavelength is 526nm
Figure.
Fig. 9 is Sr in embodiment5(BO3)3Fluorescence spectra of the F:5% fluorescent powder in the case where fluorescence emission wavelengths are 315nm.
Figure 10 is Sr in embodiment5(BO3)3Fluorescence spectrum of the F:5%Bi fluorescent powder in the case where fluorescence exciting wavelength is 526nm
Figure.
Figure 11 is Sr in embodiment5(BO3)3Fluorescence spectrum of the F:7%Bi fluorescent powder in the case where fluorescence emission wavelengths are 315nm
Figure.
Figure 12 is Sr in embodiment5(BO3)3Fluorescence spectrum of the F:7%Bi fluorescent powder in the case where fluorescence exciting wavelength is 526nm
Figure.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
A kind of preparation method of Bi doping borofluoride, comprising the following steps:
(1) according to chemical formula Sr5(BO3)3The stoichiometric ratio of each element in F:1%Bi, preparation total amount are the glimmering of 1mmol
Light powder.Strontium carbonate SrCO is weighed respectively34.99mmol, boric acid H3BO31mmol, strontium fluoride SrF21mmol adulterates bismuth oxide
Bi2O31%.
(2) by weighed strontium carbonate SrCO3, boric acid H3BO3, strontium fluoride SrF2, bismuth oxide Bi2O3In agate mortar,
Grinding 20 minutes, then mixed powder is moved in crucible, it places into high-temperature calcination stove and is pre-sintered, pre-sintering temperature is
550 DEG C, the pre-sintering time is 7h.
(3) after being cooled to room temperature to gained agglutinating matter, taking-up obtained material, which is placed again into agate mortar, grinds 10
Minute, it is uniformly mixed and is followed by sintered 7h at 1050 DEG C, cooled to room temperature is sintered 8h at 1050 DEG C again.
(4) it by gains cooled to room temperature, is finally fully ground to powder, Sr can be obtained5(BO3)3F:1%Bi
Fluorescent powder (Bi adulterates borofluoride).
Sr in the present embodiment5(BO3)3The XRD spectrum of F:1%Bi fluorescent powder is as shown in Figure 1.Fluorescence spectra such as Fig. 5 is (glimmering
Light emitting wavelength is shown in 315nm), Fig. 6 (fluorescence exciting wavelength 526nm).
Embodiment 2:
A kind of preparation method of Bi doping borofluoride, comprising the following steps:
(1) according to chemical formula Sr5(BO3)3The stoichiometric ratio of each element in F:1%Bi, preparation total amount are the glimmering of 1mmol
Light powder.Strontium carbonate SrCO is weighed respectively34.99mmol, boric acid H3BO31mmol, strontium fluoride SrF21mmol adulterates bismuth oxide
Bi2O31%.
(2) by weighed strontium carbonate SrCO3, boric acid H3BO3, strontium fluoride SrF2, bismuth oxide Bi2O3In agate mortar,
Grinding 10 minutes, then mixed powder is moved in crucible, it places into high-temperature calcination stove and is pre-sintered, pre-sintering temperature is
500 DEG C, the pre-sintering time is 8h.
(3) it after being cooled to room temperature to gained agglutinating matter, takes out obtained material and is placed again into 5 points of grinding in agate mortar
Clock is uniformly mixed and is followed by sintered 8h at 800 DEG C, and cooled to room temperature is sintered 8h at 1000 DEG C again.
(4) it by gains cooled to room temperature, is finally fully ground to powder, Sr can be obtained5(BO3)3F:1%Bi
Fluorescent powder (Bi adulterates borofluoride).
Embodiment 3:
A kind of preparation method of Bi doping borofluoride, comprising the following steps:
(1) according to chemical formula Sr5(BO3)3The stoichiometric ratio of each element in F:1%Bi, preparation total amount are the glimmering of 1mmol
Light powder.Strontium carbonate SrCO is weighed respectively34.99mmol, boric acid H3BO31mmol, strontium fluoride SrF21mmol adulterates bismuth oxide
Bi2O31%.
(2) by weighed strontium carbonate SrCO3, boric acid H3BO3, strontium fluoride SrF2, bismuth oxide Bi2O3In agate mortar,
Grinding 30 minutes, then mixed powder is moved in crucible, it places into high-temperature calcination stove and is pre-sintered, pre-sintering temperature is
600 DEG C, the pre-sintering time is 6h.
(3) after being cooled to room temperature to gained agglutinating matter, taking-up obtained material, which is placed again into agate mortar, grinds 10
Minute, it is uniformly mixed and is followed by sintered 7.5h at 1100 DEG C, cooled to room temperature is sintered 7h at 1100 DEG C again.
(4) it by gains cooled to room temperature, is finally fully ground to powder, Sr can be obtained5(BO3)3F:1%Bi
Fluorescent powder (Bi adulterates borofluoride).
Embodiment 4:
A kind of preparation method of Bi doping borofluoride, comprising the following steps:
(1) according to chemical formula Sr5(BO3)3The stoichiometric ratio of each element in F:3%Bi, preparation total amount are the glimmering of 1mmol
Light powder.Strontium carbonate SrCO is weighed respectively34.97mmol, boric acid H3BO31mmol, strontium fluoride SrF21mmol adulterates bismuth oxide
Bi2O33%.
(2) by weighed strontium carbonate SrCO3, boric acid H3BO3, strontium fluoride SrF2, bismuth oxide Bi2O3In agate mortar,
Grinding 30 minutes, then mixed powder is moved in crucible, it places into high-temperature calcination stove and is pre-sintered, pre-sintering temperature is
700 DEG C, the pre-sintering time is 4h.
(3) after being cooled to room temperature to gained agglutinating matter, taking-up obtained material, which is placed again into agate mortar, grinds 15
Minute, it is uniformly mixed and is followed by sintered 8h at 900 DEG C, cooled to room temperature is sintered 8h at 900 DEG C again.
(4) it by gains cooled to room temperature, is finally fully ground to powder, Sr can be obtained5(BO3)3F:3.0%
Bi fluorescent powder (Bi adulterates borofluoride).
Sr in the present embodiment5(BO3)3The XRD spectrum of F:3%Bi fluorescent powder is as shown in Figure 2.Fluorescence spectra such as Fig. 7 is (glimmering
Light emitting wavelength is shown in 315nm), Fig. 8 (fluorescence exciting wavelength 526nm).
Embodiment 5:
A kind of preparation method of Bi doping borofluoride, comprising the following steps:
(1) according to chemical formula Sr5(BO3)3The stoichiometric ratio of each element in F:3%Bi, preparation total amount are the glimmering of 1mmol
Light powder.Strontium carbonate SrCO is weighed respectively34.97mmol, boric acid H3BO31mmol, strontium fluoride SrF21mmol adulterates bismuth oxide
Bi2O33%.
(2) by weighed strontium carbonate SrCO3, boric acid H3BO3, strontium fluoride SrF2, bismuth oxide Bi2O3In agate mortar,
Grinding 25 minutes, then mixed powder is moved in crucible, it places into high-temperature calcination stove and is pre-sintered, pre-sintering temperature is
650 DEG C, the pre-sintering time is 3.5h.
(3) after being cooled to room temperature to gained agglutinating matter, taking-up obtained material, which is placed again into agate mortar, grinds 15
Minute, it is uniformly mixed and is followed by sintered 7h at 1100 DEG C, cooled to room temperature is sintered 7h at 1000 DEG C again.
(4) it by gains cooled to room temperature, is finally fully ground to powder, Sr can be obtained5(BO3)3F:3%Bi
Fluorescent powder (Bi adulterates borofluoride).
Embodiment 6:
A kind of preparation method of Bi doping borofluoride, comprising the following steps:
(1) according to chemical formula Sr5(BO3)3The stoichiometric ratio of each element in F:3%Bi, preparation total amount are the glimmering of 1mmol
Light powder.Strontium carbonate SrCO is weighed respectively34.97mmol, boric acid H3BO31mmol, strontium fluoride SrF21mmol adulterates bismuth oxide
Bi2O33%.
(2) by weighed strontium carbonate SrCO3, boric acid H3BO3, strontium fluoride SrF2, bismuth oxide Bi2O3In agate mortar,
Grinding 10 minutes, then mixed powder is moved in crucible, it places into high-temperature calcination stove and is pre-sintered, pre-sintering temperature is
800 DEG C, the pre-sintering time is 3h.
(3) after being cooled to room temperature to gained agglutinating matter, taking-up obtained material, which is placed again into agate mortar, grinds 10
Minute, it is uniformly mixed and is followed by sintered 8h at 800 DEG C, cooled to room temperature is sintered 7.5h at 900 DEG C again.
(4) it by gains cooled to room temperature, is finally fully ground to powder, Sr can be obtained5(BO3)3F:3%Bi
Fluorescent powder (Bi adulterates borofluoride).
Embodiment 7:
A kind of preparation method of Bi doping borofluoride, comprising the following steps:
(1) according to chemical formula Sr5(BO3)3The stoichiometric ratio of each element in F:5%Bi, preparation total amount are the glimmering of 1mmol
Light powder.Strontium carbonate SrCO is weighed respectively34.95mmol, boric acid H3BO31mmol, strontium fluoride SrF21mmol adulterates bismuth oxide
Bi2O35%.
(2) by weighed strontium carbonate SrCO3, boric acid H3BO3, strontium fluoride SrF2, bismuth oxide Bi2O3In agate mortar,
Grinding 10 minutes, then mixed powder is moved in crucible, it places into high-temperature calcination stove and is pre-sintered, pre-sintering temperature is
600 DEG C, the pre-sintering time is 7h.
(3) it after being cooled to room temperature to gained agglutinating matter, takes out obtained material and is placed again into 5 points of grinding in agate mortar
Clock is uniformly mixed and is followed by sintered 7h at 1250 DEG C, and cooled to room temperature is sintered 7h at 1250 DEG C again.
(4) it by gains cooled to room temperature, is finally fully ground to powder, Sr can be obtained5(BO3)3F:5.0%
Bi fluorescent powder (Bi adulterates borofluoride).
Sr in the present embodiment5(BO3)3The XRD spectrum of F:5%Bi fluorescent powder is as shown in Figure 3.Fluorescence spectra such as Fig. 9 is (glimmering
Light emitting wavelength is shown in 315nm), Figure 10 (fluorescence exciting wavelength 526nm).
Embodiment 8:
A kind of preparation method of Bi doping borofluoride, comprising the following steps:
(1) according to chemical formula Sr5(BO3)3The stoichiometric ratio of each element in F:5%Bi, preparation total amount are the glimmering of 1mmol
Light powder.Strontium carbonate SrCO is weighed respectively34.95mmol, boric acid H3BO31mmol, strontium fluoride SrF21mmol adulterates bismuth oxide
Bi2O35%.
(2) by weighed strontium carbonate SrCO3, boric acid H3BO3, strontium fluoride SrF2, bismuth oxide Bi2O3In agate mortar,
Grinding 40 minutes, then mixed powder is moved in crucible, it places into high-temperature calcination stove and is pre-sintered, pre-sintering temperature is
530 DEG C, the pre-sintering time is 6h.
(3) after being cooled to room temperature to gained agglutinating matter, taking-up obtained material, which is placed again into agate mortar, grinds 20
Minute, it is uniformly mixed and is followed by sintered 6h at 1150 DEG C, cooled to room temperature is sintered 6h at 1200 DEG C again.
(4) it by gains cooled to room temperature, is finally fully ground to powder, Sr can be obtained5(BO3)3F:5.0%
Bi fluorescent powder (Bi adulterates borofluoride).
Embodiment 9:
A kind of preparation method of Bi doping borofluoride, comprising the following steps:
(1) according to chemical formula Sr5(BO3)3The stoichiometric ratio of each element in F:5%Bi, preparation total amount are the glimmering of 1mmol
Light powder.Strontium carbonate SrCO is weighed respectively34.95mmol, boric acid H3BO31mmol, strontium fluoride SrF21mmol adulterates bismuth oxide
Bi2O35%.
(2) by weighed strontium carbonate SrCO3, boric acid H3BO3, strontium fluoride SrF2, bismuth oxide Bi2O3In agate mortar,
Grinding 35 minutes, then mixed powder is moved in crucible, it places into high-temperature calcination stove and is pre-sintered, pre-sintering temperature is
500 DEG C, the pre-sintering time is 8h.
(3) after being cooled to room temperature to gained agglutinating matter, taking-up obtained material, which is placed again into agate mortar, grinds 10
Minute, it is uniformly mixed and is followed by sintered 7h at 1100 DEG C, cooled to room temperature is sintered 6h at 1120 DEG C again.
(4) it by gains cooled to room temperature, is finally fully ground to powder, Sr can be obtained5(BO3)3F:5.0%
Bi fluorescent powder (Bi adulterates borofluoride).
Embodiment 10:
A kind of preparation method of Bi doping borofluoride, comprising the following steps:
(1) according to chemical formula Sr5(BO3)3The stoichiometric ratio of each element in F:7%Bi, preparation total amount are the glimmering of 1mmol
Light powder.Strontium carbonate SrCO is weighed respectively34.93mmol, boric acid H3BO31mmol, strontium fluoride SrF21mmol adulterates bismuth oxide
Bi2O37%.
(2) by weighed strontium carbonate SrCO3, boric acid H3BO3, strontium fluoride SrF2, bismuth oxide Bi2O3In agate mortar,
Grinding 20 minutes, then mixed powder is moved in crucible, it places into high-temperature calcination stove and is pre-sintered, pre-sintering temperature is
550 DEG C, the pre-sintering time is 7h.
(3) after being cooled to room temperature to gained agglutinating matter, taking-up obtained material, which is placed again into agate mortar, grinds 5-
It 20 minutes, is uniformly mixed and is followed by sintered 5h at 1200 DEG C, cooled to room temperature is sintered 5h at 1200 DEG C again.
(4) it by gains cooled to room temperature, is finally fully ground to powder, Sr can be obtained5(BO3)3F:7.0%
Bi fluorescent powder (Bi adulterates borofluoride).
Sr in the present embodiment5(BO3)3The XRD spectrum of F:7%Bi fluorescent powder is as shown in Figure 1.Fluorescence spectra such as Figure 11 is (glimmering
Light emitting wavelength is shown in 315nm), Figure 12 (fluorescence exciting wavelength 526nm).
Embodiment 11:
A kind of preparation method of Bi doping borofluoride, comprising the following steps:
(1) according to chemical formula Sr5(BO3)3The stoichiometric ratio of each element in F:7%Bi, preparation total amount are the glimmering of 1mmol
Light powder.Strontium carbonate SrCO is weighed respectively34.93mmol, boric acid H3BO31mmol, strontium fluoride SrF21mmol adulterates bismuth oxide
Bi2O37%.
(2) by weighed strontium carbonate SrCO3, boric acid H3BO3, strontium fluoride SrF2, bismuth oxide Bi2O3In agate mortar,
Grinding 20 minutes, then mixed powder is moved in crucible, it places into high-temperature calcination stove and is pre-sintered, pre-sintering temperature is
520 DEG C, the pre-sintering time is 6h.
(3) after being cooled to room temperature to gained agglutinating matter, taking-up obtained material, which is placed again into agate mortar, grinds 5-
It 20 minutes, is uniformly mixed and is followed by sintered 5h at 1400 DEG C, cooled to room temperature is sintered 5h at 1400 DEG C again.
(4) it by gains cooled to room temperature, is finally fully ground to powder, Sr can be obtained5(BO3)3F:7.0%
Bi fluorescent powder (Bi adulterates borofluoride).
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (6)
1. a kind of preparation method of Bi doping borofluoride, which comprises the following steps:
(1) it is pre-sintered: weighing SrCO respectively by raw material proportioning3、SrF2、H3BO3、Bi2O3It is ground in agate mortar, then will mixing
Powder move in crucible, and be put into high-temperature calcination stove and be pre-sintered, pre-sintering temperature is 500-800 DEG C, when pre-sintering
Between be 3-7h；
(2) after agglutinating matter obtained by handling through step (1) is cooled to room temperature, gains the preparation of fluorescent powder: are taken out again
It is put into agate mortar and grinds, be sintered 5-8h, cooled to room temperature, again in 800- at 800-1400 DEG C after mixing
5-8h is sintered at 1400 DEG C；Gains cooled to room temperature, and it is ground to powder, Bi doping borofluoride Sr can be obtained5
(BO3)3F:x%Bi, wherein 0.01≤x≤15.
2. the preparation method of Bi doping borofluoride according to claim 1, which is characterized in that wherein, 0.5≤x≤10.
3. the preparation method of Bi doping borofluoride according to claim 2, which is characterized in that wherein, 1≤x≤7.
4. the preparation method of Bi doping borofluoride according to claim 3, which is characterized in that when 1≤x≤3, the step
Suddenly in (2), sintering temperature is 800-1100 DEG C, sintering time 7-8h, cooled to room temperature, again at 800-1100 DEG C
It is sintered 7-8h；When 3≤x≤7, in the step (2), sintering temperature is 1100-1400 DEG C, and time 5-7h is naturally cooled to
Room temperature is sintered 5-7h at 1100-1400 DEG C again.
5. the preparation method of Bi doping borofluoride according to claim 1, which is characterized in that in the step (1), in
It is ground 10-40 minutes in agate mortar.
6. the preparation method of Bi doping borofluoride according to claim 1, which is characterized in that in the step (2), take
Gains are placed again into agate mortar and grind 5-20 minutes out.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2762551C1 (en) * | 2021-04-19 | 2021-12-21 | Федеральное государственное бюджетное учреждение науки Институт химии Дальневосточного отделения Российской академии наук (ИХ ДВО РАН) | Method for obtaining lanthanum orthoborates doped with europium and bismuth |
| CN114276012A (en) * | 2020-09-28 | 2022-04-05 | 天津工业大学 | Rare earth element Dy-doped fluoborate luminescent glass and preparation method thereof |
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2019
- 2019-09-04 CN CN201910833643.7A patent/CN110499154A/en active Pending
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114276012A (en) * | 2020-09-28 | 2022-04-05 | 天津工业大学 | Rare earth element Dy-doped fluoborate luminescent glass and preparation method thereof |
| CN114276012B (en) * | 2020-09-28 | 2023-12-01 | 天津工业大学 | Rare earth element Dy doped fluoborate luminescent glass and preparation method thereof |
| RU2762551C1 (en) * | 2021-04-19 | 2021-12-21 | Федеральное государственное бюджетное учреждение науки Институт химии Дальневосточного отделения Российской академии наук (ИХ ДВО РАН) | Method for obtaining lanthanum orthoborates doped with europium and bismuth |
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Application publication date: 20191126 |