CN107235496A - A kind of Firebrake ZB ZnB2O4The low temperature preparation method of luminescent material - Google Patents
A kind of Firebrake ZB ZnB2O4The low temperature preparation method of luminescent material Download PDFInfo
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- CN107235496A CN107235496A CN201710549987.6A CN201710549987A CN107235496A CN 107235496 A CN107235496 A CN 107235496A CN 201710549987 A CN201710549987 A CN 201710549987A CN 107235496 A CN107235496 A CN 107235496A
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- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/63—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing boron
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Abstract
The present invention discloses a kind of Firebrake ZB ZnB2O4The low temperature preparation method of luminescent material, comprises the following steps：1) zinc source and boron source are weighed respectively；2) sample weighed up is well mixed, adds distilled water, obtain mixture；3) mixture is obtained into white solid in carrying out water bath processing at 60 100 DEG C 10 hours；The white solid of gained is washed 36 times repeatedly with distilled water, ethanol, drying obtains predecessor in 12 hours at 60 DEG C afterwards；4) predecessor is obtained into target product Firebrake ZB ZnB in carrying out roasting 25 hours at 500 700 DEG C after cooling2O4.This method is simple and quick, and environmental protection, production cost is low, and low energy consumption, and the product optical purity prepared by it is high, and monochromaticjty is good.
Description
Technical field
The invention belongs to field of inorganic materials, and in particular to a kind of Firebrake ZB ZnB2O4The low temperature preparation method of luminescent material.
Background technology
Firebrake ZB ZnB2O4In boron atom B use SP2Hybrid form and three oxygen atom O formation have plane triangle
The borate ion BO of structure3 3-, thus with excellent chemical stability and optical stability, obtain extensive concern.
At present, on Firebrake ZB ZnB2O4Preparation method be mainly high temperature solid-state method, this method it is general with ZnO,
H3BO3For raw material, by 1:2 ratio is fully ground after mixing, is calcined and is made at 900 DEG C.Product made from this preparation method
Purity is not high, and particle agglomeration is serious, it is impossible to keeps the homogeneity of the homogeney, the physical property of particle and particle diameter of product well,
Moreover high temperature power consumption cost, therefore the calcining heat of reduction high temperature solid state reaction, it is cost-effective, energy consumption is reduced, Firebrake ZB is improved
ZnB2O4Purity, homogeneity is very important.
Firebrake ZB ZnB2O4Inherently a kind of inorganic fluorescent material of blue light-emitting, it is not necessary to which adulterate any rare earth element, gold
Belong to element, so as to greatly reduce cost and energy consumption.Therefore, its purity is improved, it can be extended in terms of luminescent material
Using range, actual demand can be more met.
The content of the invention
Present invention aims at provide a kind of Firebrake ZB ZnB2O4The low temperature preparation method of luminescent material, passes through simple side
Method, cheap raw material efficiently and rapidly prepares the Firebrake ZB inorganic fluorescent material with good luminous performance, products obtained therefrom hair
Optical purity is high, and monochromaticjty is good, and production cost is low, and synthetic method is simple and quick, and environmental protection, low energy consumption.
The present invention for reach technical scheme that above-mentioned purpose used for：
A kind of Firebrake ZB ZnB2O4The low temperature preparation method of luminescent material, comprises the following steps：
1) a certain proportion of zinc source and boron source are weighed respectively；
2) sample weighed up is well mixed, adds distilled water, obtain mixture；
3) mixture is subjected to water bath processing 10 hours, obtains white solid；By the white solid distilled water of gained, second
Alcohol is washed 3-6 times repeatedly, and drying obtains predecessor in 12 hours at 60 DEG C afterwards；
4) predecessor is obtained into target product Firebrake ZB in carrying out roasting 2-5 hours at 500-700 DEG C after cooling
ZnB2O4。
Described low temperature preparation method, the zinc source be zinc sulfate, zinc nitrate, zinc chloride, zinc carbonate, basic zinc carbonate or
Zinc acetate.
Described low temperature preparation method, the boron source is boric acid or borax.
A kind of described Firebrake ZB ZnB2O4The low temperature preparation method of luminescent material, step 1) in zinc source and boron source mole
Than for 2:0.8-1.2.
Described low temperature preparation method, step 2) be specially：Under stirring, stirred toward one equipped with condenser pipe and machinery
Mix and distilled water, zinc source and boron source are added in the three-neck flask of device, mixture is obtained after mixing.
Described low temperature preparation method step 3) in mixture bath temperature be 60-100 DEG C.
Described low temperature preparation method, step 4) in sintering temperature be 500-700 DEG C, roasting heating rate is on per minute
Rise 5 DEG C
The Firebrake ZB ZnB prepared using described low temperature preparation method2O4Application on as blue emitting material.
The beneficial effects of the invention are as follows：
A kind of Firebrake ZB ZnB of blue light-emitting is provided2O4Low temperature preparation method, by water bath processing, what low-temperature bake was obtained
Sample monochromaticjty is good, can send purer blue light.Present invention process is easily controllable, simple to operate, short preparation period, production cost
Low, good product quality, is adapted to large-scale industrial production.
The present invention will obtain predecessor using borax (boric acid) and zinc salt as raw material after raw material mixing heating water bath, by before
Drive thing to be calcined in the case of not higher than 700 DEG C, obtain ZnB2O4.The preparing raw material of the present invention is cheap and easy to get, simple to operate, green
Environmental protection, efficiently can quickly synthesize ZnB2O4, and the ZnB prepared compared to conventional high-temperature solid phase method2O4Sintering temperature is significantly
Reduction, has saved cost, has reduced energy consumption, improved efficiency, what is more important maintains ZnB well2O4Basic Physical Properties
With uniform particle diameter, luminous intensity is improved.ZnB prepared by the method2O4Can also may be used as a kind of potential blue emitting material
Preparation applied to white light LEDs.
Brief description of the drawings
Fig. 1 is Firebrake ZB ZnB2O4Infrared spectrogram, wherein (a) be embodiment 3 obtained by Firebrake ZB ZnB2O4, (b)
The ZnB made from conventional high-temperature solid phase method in contrast experiment2O4。
Fig. 2 is Firebrake ZB ZnB2O4X-ray powder diffraction collection, wherein (a) be embodiment 3 obtained by Firebrake ZB
ZnB2O4, (b) is the ZnB obtained by conventional high-temperature solid phase method in contrast experiment2O4。
Fig. 3 a are the Firebrake ZB ZnB obtained by embodiment 32O4ESEM collection of illustrative plates.
Fig. 3 b are ZnB made from conventional high-temperature solid phase method in contrast experiment2O4ESEM collection of illustrative plates.
Fig. 4 is Firebrake ZB ZnB2O4Transmitting collection of illustrative plates, (a) is the Firebrake ZB ZnB of the gained of embodiment 32O4, (b) is real for contrast
Test ZnB made from conventional high-temperature solid phase method2O4。
Fig. 5 is the Firebrake ZB ZnB of the gained of embodiment 32O4CIE chromaticity coordinates figures.
Embodiment
With reference to embodiments, the present invention is further described in detail, but is not limited to this.Adopted in the following example
Chemicals is all commercial chemicals.
A kind of Firebrake ZB ZnB of embodiment 12O4The low temperature preparation method of luminescent material
Step is as follows：
1) 3.8137g Na are weighed respectively2B4O7·10H2O, 2.9751g Zn (NO3)2·6H2O。
2) by the sample weighed up under stirring, a three-neck flask equipped with condenser pipe and mechanical agitator is added
In, and 100mL distilled water is added, obtain a kind of mixture.
3) mixture is obtained into white solid in water-bath 10 hours at 80 DEG C.By the white solid distilled water of gained, second
Alcohol is washed 3-6 times repeatedly, and drying obtains predecessor in 12 hours at 60 DEG C afterwards.
4) predecessor is calcined 3 hours at 500 DEG C, heating rate rises 5 DEG C to be per minute, and mesh is can obtain after cooling
Mark product.
A kind of Firebrake ZB ZnB of embodiment 22O4The low temperature preparation method of luminescent material
Only change step 4) in sintering temperature, i.e., predecessor is calcined 3 hours at 600 DEG C；Other steps are with implementation
Example 1, is made target product.
A kind of Firebrake ZB ZnB of embodiment 32O4The low temperature preparation method of luminescent material
Only change step 4) in sintering temperature, i.e., predecessor is calcined 3 hours at 700 DEG C；Other steps are with implementation
Example 1, is made target product.
Sintering temperature is to Firebrake ZB ZnB2O4The influence of luminescent material：From embodiment 1-3, when sintering temperature is 700 DEG C
When, obtained Firebrake ZB ZnB2O4Powder diameter is more homogeneous, and purity is higher.It is therefore preferable that Firebrake ZB ZnB2O4Optimal roasting
It is 700 DEG C to burn temperature.
A kind of Firebrake ZB ZnB of embodiment 42O4The low temperature preparation method of luminescent material
Only change step 4) in roasting time, i.e., predecessor is calcined 2 hours at 700 DEG C；Other steps are with implementation
Example 3, is made target product.
A kind of Firebrake ZB ZnB of embodiment 52O4The low temperature preparation method of luminescent material
Only change step 4) in roasting time, i.e., predecessor is calcined 4 hours at 700 DEG C；Other steps are with implementation
Example 3, is made target product.
A kind of Firebrake ZB ZnB of embodiment 62O4The low temperature preparation method of luminescent material
Only change step 4) in roasting time, i.e., predecessor is calcined 5 hours at 700 DEG C；Other steps are with implementation
Example 3, is made target product.
Roasting time is to Firebrake ZB ZnB2O4The influence of luminescent material：From embodiment 3-6, upon firing between be 3 hours
When, obtained ZnB2O4Preferably, structure is homogeneous for crystal formation, extends roasting time not only time consumption and energy consumption, and can cause product
Reunite, product purity reduction, luminescent properties weaken.It is therefore preferable that roasting time is 3 hours.
A kind of Firebrake ZB ZnB of embodiment 72O4The low temperature preparation method of luminescent material
Only change step 3) in bath temperature, i.e., mixture is obtained into white solid in water-bath 10 hours at 60 DEG C.Its
His step be the same as Example 3, is made target product.
A kind of Firebrake ZB ZnB of embodiment 82O4The low temperature preparation method of luminescent material
Only change step 3) in bath temperature, i.e., mixture is obtained into white solid in water-bath 10 hours at 70 DEG C.Its
His step be the same as Example 3, is made target product.
A kind of Firebrake ZB ZnB of embodiment 92O4The low temperature preparation method of luminescent material
Only change step 3) in bath temperature, i.e., mixture is obtained into white solid in water-bath 10 hours at 90 DEG C.Its
His step be the same as Example 3, is made target product.
A kind of Firebrake ZB ZnB of embodiment 102O4The low temperature preparation method of luminescent material
Only change step 3) in bath temperature, i.e., mixture is obtained into white solid in water-bath 10 hours at 100 DEG C.
Other step be the same as Examples 3, are made target product.
Bath temperature is to Firebrake ZB ZnB2O4The influence of luminescent material：From embodiment 3,7-10, when bath temperature is 80
DEG C when, it is higher to react obtained white solid yield, illustrate 80 DEG C for preferred bath temperature.
A kind of Firebrake ZB ZnB of embodiment 112O4The low temperature preparation method of luminescent material
Only change step 1) in zinc source and boron source mol ratio, i.e. Na2B4O7·10H2O and Zn (NO3)2·6H2O mole
Than for 2:0.8.Other step be the same as Examples 3, are made target product.
A kind of Firebrake ZB ZnB of embodiment 122O4The low temperature preparation method of luminescent material
Only change step 1) in zinc source and boron source mol ratio, i.e. Na2B4O7·10H2O and Zn (NO3)2·6H2O mole
Than for 2:1.2.Other step be the same as Examples 3, are made target product.
Different zinc sources and the mol ratio of boron source are to Firebrake ZB ZnB2O4The influence of luminescent material：Can by embodiment 3,11-12
Know, when the mol ratio of zinc source and boron source is 2:What zinc source and boron source were reacted when 1 is more complete, obtained white solid impurity compared with
Few, yield is higher, and sample purity is also of a relatively high.
A kind of Firebrake ZB ZnB of embodiment 132O4The low temperature preparation method of luminescent material
Only change step 1) in zinc salt species and consumption, that is, weigh 2.8758g ZnSO4·7H2O, other steps are same
Embodiment 3, is made target product.
A kind of Firebrake ZB ZnB of embodiment 142O4The low temperature preparation method of luminescent material
Only change step 1) in zinc salt species and consumption, that is, weigh 1.2542g ZnCO3, other step be the same as Examples
3, target product is made.
Different zinc salts is to Firebrake ZB ZnB2O4The influence of luminescent material：From embodiment 3,13-14, when selecting Zn
(NO3)2·6H2When O is reaction raw materials, bath temperature is that 80 DEG C of obtained white solid yields are higher；When selecting ZnSO4·7H2O
During for reaction raw materials, bath temperature is that 100 DEG C or so yields are preferable；When selecting ZnCO3During for reaction raw materials, bath temperature is 70
DEG C or so yield it is preferable.In view of bath temperature and cost of material, zinc salt preferably is Zn (NO3)2·6H2O。
The contrast experiment of embodiment 15
4.0704g ZnO, 6.1833g H are weighed respectively3BO3It is placed in mortar and grinds half an hour to uniformly mixing, afterwards
It is placed in Muffle furnace at 900 DEG C and is calcined 6 hours, heating rate rises 5 DEG C to be per minute, and cooling can obtain product (b).
It can be seen from figure 1 that compound b is the ZnB obtained by conventional high-temperature solid phase2O4, its characteristic absorption peak is belonged to：
1090cm-1Place is attributed to three-fold coordination boron oxygen key (B(3)- O) asymmetric stretching vibration；955cm-1Place is attributed to (B(3)- O) it is non-
It is symmetrical flexible；722cm-1Place is attributed to (B(3)- O) out-of-plane bending；478cm-1Place is attributed to Zn-O bending；Show in compound
Only exist-BO3, not comprising-BO4ZnB in group, with document2O4Characteristic absorption peak it is consistent, it is ZnB to show compound b2O4It is pure
Phase.Compound a shown in figure is the Firebrake ZB ZnB obtained by embodiment 32O4Infrared spectrum characteristic absorption peak and ZnB2O4
Pure phase it is basically identical, illustrate compound a also be ZnB2O4Pure phase.
Fig. 2 is Firebrake ZB ZnB of the compound a obtained by embodiment 32O4It is conventional high-temperature in contrast experiment with compound b
ZnB obtained by solid phase method2O4XRD spectra, the ZnB provided in its XRD spectra shown in figure and document2O4Standard PDF cards
Unanimously, other miscellaneous peaks are not observed in piece (JCPDS 39-1126), and that this shows to obtain under the present conditions is ZnB2O4It is pure
Phase, and the crystallinity of compound a is higher than compound b crystallinity.
Fig. 3 a and Fig. 3 b are the Firebrake ZB ZnB obtained by compound a embodiment 3 respectively2O4In compound b contrast experiments
ZnB obtained by conventional high-temperature solid phase method2O4Scanning electron microscope (SEM) photograph.It can be observed from figure, compound a is by irregular circle
Constituted with square particle, average diameter is about in 0.5-0.6um or so, and relative to compound b, and the particle diameter of compound a is more equal
One, ZnB can be kept well2O4Homogeney, the physical property of particle, illustrate this method synthesis ZnB2O4Purity is higher.
Fig. 4 is the Firebrake ZB ZnB obtained by the compound a embodiment 3 under the monitoring of 310nm excitation wavelengths2O4With compound b
ZnB in contrast experiment obtained by conventional high-temperature solid phase method2O4Emission spectrum, wave-length coverage is 350-500nm.Can from figure
To find out, compound has a strong emission peak at 392nm, and luminous intensity is respectively 2234au and 1205au, explanation
Compound can launch good blue light.And the luminous intensity of compound a illustrates the change of method synthesis apparently higher than compound b
The luminous intensity of compound is higher, and monochromaticjty is more preferable.
Fig. 5 is the Firebrake ZB ZnB obtained by compound a embodiment 32O4CIE chromaticity coordinates figures, chromaticity coordinates for (0.1514,
0.0365), it is also seen that compound a is in the higher blue region of purity from figure.
Claims (8)
1. a kind of Firebrake ZB ZnB2O4The low temperature preparation method of luminescent material, it is characterised in that comprise the following steps：
1) zinc source and boron source are weighed respectively；
2) sample weighed up is well mixed, adds distilled water, obtain mixture；
3) mixture is subjected to water bath processing 10 hours, obtains white solid；White solid distilled water, the ethanol of gained is anti-
After backwashing 3-6 times, drying obtains predecessor in 12 hours at 60 DEG C afterwards；
4) predecessor is obtained into target product Firebrake ZB ZnB in carrying out roasting 2-5 hours at 500-700 DEG C after cooling2O4。
2. low temperature preparation method according to claim 1, it is characterised in that the zinc source is zinc sulfate, zinc nitrate, chlorination
Zinc, zinc carbonate, basic zinc carbonate or zinc acetate.
3. low temperature preparation method according to claim 1, it is characterised in that the boron source is boric acid or borax.
4. a kind of Firebrake ZB ZnB according to claim 12O4The low temperature preparation method of luminescent material, it is characterised in that step
It is rapid 1) in zinc source and boron source mol ratio be 2:0.8-1.2.
5. low temperature preparation method according to claim 1, it is characterised in that step 2) be specially：It is past under stirring
Distilled water, zinc source and boron source are added in one three-neck flask equipped with condenser pipe and mechanical agitator, mixture is obtained after mixing.
6. low temperature preparation method according to claim 1, it is characterised in that step 3) in the bath temperature of mixture be
60-100℃。
7. low temperature preparation method according to claim 1, it is characterised in that step 4) in sintering temperature be 500-700 DEG C,
It is calcined heating rate and rises 5 DEG C to be per minute.
8. the Firebrake ZB ZnB prepared using the low temperature preparation method described in claim 1-72O4On as blue emitting material
Application.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780962A (en) * | 2010-04-01 | 2010-07-21 | 山东川君化工股份有限公司 | Method for preparing decahydrate zinc borate |
| CN102502680A (en) * | 2011-10-13 | 2012-06-20 | 北京石油化工学院 | Method for preparing sub-micron zinc borate by using glycerol |
| CN104073252A (en) * | 2014-06-06 | 2014-10-01 | 陕西师范大学 | Preparation method of ZnB2O4:Eu<3+> luminescent material |
| CN106219565A (en) * | 2016-07-25 | 2016-12-14 | 淄博五维实业有限公司 | The preparation method of three hydrate zinc borates |
-
2017
- 2017-07-07 CN CN201710549987.6A patent/CN107235496A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780962A (en) * | 2010-04-01 | 2010-07-21 | 山东川君化工股份有限公司 | Method for preparing decahydrate zinc borate |
| CN102502680A (en) * | 2011-10-13 | 2012-06-20 | 北京石油化工学院 | Method for preparing sub-micron zinc borate by using glycerol |
| CN104073252A (en) * | 2014-06-06 | 2014-10-01 | 陕西师范大学 | Preparation method of ZnB2O4:Eu<3+> luminescent material |
| CN106219565A (en) * | 2016-07-25 | 2016-12-14 | 淄博五维实业有限公司 | The preparation method of three hydrate zinc borates |
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| NIL KUCUK ET AL.: "Synthesis,thermoluminescence and dosimetric properties of La-doped zinc borates", 《JOURNAL OF LUMINESCENCE》 * |
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Application publication date: 20171010 |