CN106147756A - A kind of mechanoluminescence red fluorescence powder and preparation method thereof - Google Patents
A kind of mechanoluminescence red fluorescence powder and preparation method thereof Download PDFInfo
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- CN106147756A CN106147756A CN201610509126.0A CN201610509126A CN106147756A CN 106147756 A CN106147756 A CN 106147756A CN 201610509126 A CN201610509126 A CN 201610509126A CN 106147756 A CN106147756 A CN 106147756A
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- mechanoluminescence
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/57—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing manganese or rhenium
- C09K11/572—Chalcogenides
- C09K11/576—Chalcogenides with alkaline earth metals
Abstract
The invention discloses a kind of mechanoluminescence red fluorescence powder, expressing formula is BaZn(1‑x)OS:xMn2+, wherein 0.1%≤x≤1.0%, active ions are Mn2+Ion.The invention also discloses the preparation method of above-mentioned mechanoluminescence red fluorescence powder: (1) weighs containing barium compound, sulfur-containing compound, zinc compound respectively and contains manganese compound as raw material；(2), after the raw materials of compound weighing step (1) grinds uniformly, roasting under protective atmosphere or vacuum, temperature is 900～1100 DEG C, and the time is 2～10 hours；(3) sample after roasting in step (2) is taken out, grind and i.e. obtain mechanoluminescence red fluorescence powder.The mechanoluminescence red fluorescence powder of the present invention to mechanical force stimulate obvious response to, tribo-luminescence naked eyes on daytime are visible, and with low cost, preparation process is simple.
Description
Technical field
The present invention relates to luminescent material, particularly to a kind of mechanoluminescence red fluorescence powder and preparation method thereof.
Background technology
The mensuration of stress intensity and distribution suffered by material structure component, to improving Member Reliability Analysis and security, expands it
For application of crucial importance.The technology of existing several typical detection stress intensity has resistance-strain Pressure gauge, piezoelectricity
Formula sensor etc..These technology use the signal of telecommunication as detection signal, collect necessary holding electrode during signal good with tested position
Good physical contact, is therefore only used for stationary parts, is difficult to measure stress intensity suffered by cutting element or gas turbine.Additionally,
Due to the restriction of size sensor and measurement point, they are not suitable for measuring stress distribution.At present, utilize optical fiber sensing technology permissible
Realizing that stress distribution measures, this technology needs to be covered with optical fiber detected material, and requires that the laser work providing optical signal is stable,
Once optical fiber is impaired, and whole sensor-based system can not work, and needs to rearrange fibre system.Additionally, utilize Fibre Optical Sensor skill
Art process is loaded down with trivial details, and cost is high, is not suitable for the real time health detection of material structure.
Therefore a kind of visualization technique of development, can monitor stress size and be distributed of crucial importance in real time, the pass of this technology
Key is discovery mechanoluminescence new material, and this material can be luminous under the effect of mechanical force, and luminous intensity is big with stress
Little proportional.Utilize mechanoluminescence material as stress pop one's head in, in conjunction with CCD imaging technique, it is achieved to material structure parts,
The stress distribution of bridge, dam or high-rise and the real-time monitoring of size.The mechanoluminescence material of report is mainly at present
Rear-earth-doped aluminate materials, its luminescence is positioned at green-yellow light wave band, does not has luminescence in more long-wave band.
Content of the invention
In order to overcome disadvantages mentioned above and the deficiency of prior art, it is an object of the invention to provide a kind of mechanoluminescence red
Emitting red light under ultraviolet excitation for the fluorescent material covers the spectral regions of 550～800nm, the mechanoluminescence under frictional force excites
Covering the spectral regions of 500～700nm, the mechanoluminescence under pressure excites covers the spectral regions of 550～700nm.
Another object of the present invention is to provide the preparation method of above-mentioned mechanoluminescence red fluorescence powder, preparation process does not relates to
And harmful material, preparation process is simple, it is simple to volume production.
The purpose of the present invention is achieved through the following technical solutions:
A kind of mechanoluminescence red fluorescence powder, expressing formula is BaZn(1-x)OS:xMn2+, wherein 0.1%≤x≤1.0%,
Active ions are Mn2+Ion.
Described mechanoluminescence red fluorescence powder, works as x=0.5%, and tribo-luminescence and pressure illumination effect are optimal.
The preparation method of a kind of mechanoluminescence red fluorescence powder, comprises the following steps:
(1) each element mol ratio Ba:Zn:S:Mn=1:1:1:x is pressed；Weigh respectively containing barium compound, sulfur-containing compound,
Zinc compound and containing manganese compound as raw material；0.1%≤x≤1.0%；
(2) after the raw materials of compound weighing step (1) grinds uniformly, roasting under protective atmosphere or vacuum, temperature
Being 900～1100 DEG C, the time is 2～10 hours；
(3) sample after roasting in step (2) is taken out, grind and i.e. obtain mechanoluminescence red fluorescence powder.
Described protective atmosphere is argon gas atmosphere or nitrogen atmosphere.
As x=0.5%, being roasted to 1050 DEG C, illumination effect is optimal.
Described containing barium compound is brium carbonate, barium monoxide, the one in barium hydroxide.
Described sulfur-containing compound is zinc sulphide.
Described zinc compound is zinc sulphide.
Described is any one in manganous oxide, manganese oxide, manganese dioxide and manganese carbonate containing manganese compound.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) emitting red light under ultraviolet excitation for the mechanoluminescence red fluorescence powder of the present invention covers 550～800nm's
Spectral regions, the mechanoluminescence under frictional force excites covers the spectral regions of 500～700nm, the mechanoluminescence under pressure excites
Cover the spectral regions of 550～700nm.
(2) mechanical force stimulation is obvious responsed to by the mechanoluminescence red fluorescence powder of the present invention, tribo-luminescence naked eyes on daytime
Visible, luminous intensity and stress intensity are good linear relation.
(3) preparation method of the mechanoluminescence red fluorescence powder of the present invention, preparation technology is simple, and one-step method is burnt till, temperature
Condition (900～1100 DEG C) is easier to realize.
(4) present invention is on raw material selects, and uses cheap transient metal Mn to replace rare earths material as the centre of luminescence, system
Standby process is not related to toxic corrosive raw material.
Brief description
Fig. 1 is sample powder x-ray diffraction spectrum under different temperatures gradient roasting in embodiment 1.
Fig. 2 is emission spectrum under different temperatures gradient roasting for the sample in embodiment 1.
Fig. 3 is excitation spectrum under different temperatures gradient roasting for the sample in embodiment 1.
Fig. 4 is the tribo-luminescence spectrum of sample in embodiment 2.
Fig. 5 is luminescent spectrum under sample different size pressure in embodiment 3.
Fig. 6 is luminous intensity and the pressure magnitude relationship matched curve of sample in embodiment 3.
Fig. 7 is the luminescent spectrum figure of sample under different mode of excitation in embodiment 3.
Fig. 8 is the different influence curves to luminous intensity for the Mn ion concentration in embodiment 4.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
Choose brium carbonate, zinc sulphide, manganese carbonate as raw material, according to mol ratio Ba:Zn:S:Mn=1:1:1:0.005, claim
Take brium carbonate, zinc sulphide, manganese carbonate are respectively 3.3407g, 1.6496g, 0.0097g.Raw material is ground mix after, take in right amount in
In corundum crucible, then crucible is placed in corundum boat, corundum boat is pushed in tube furnace, under argon gas atmosphere respectively at 1000 DEG C,
1050 DEG C, 1100 DEG C of roastings 3 hours, cool down naturally with stove, mechanoluminescence red fluorescence powder BaZn0.995OS:0.5%
Mn2+。
Fig. 1 is the powder x-ray diffraction spectrum of the sample of roasting under the present embodiment different temperatures, and spectral line uses Japan
Rigaku D/max-IIIA X-ray diffractometer measures, test voltage 40kV, 1.2 °/min of sweep speed, tests electric current 40mA,
Selecting Cu-K α 1X ray, wavelength isX-ray diffraction analysis shows all may be used at 1000 DEG C, 1050 DEG C, 1100 DEG C
To obtain BaZnOS phase, belonging to rhombic system, the doping of manganese does not affects the synthesis of crystalline phase, either with or without observing manganese and change thereof
Compound phase.But under different temperatures, sample X-ray diffraction peak relative intensity changes, with the rising of sintering temperature, permissible
See that the diffraction peak intensity of (040) crystal face dramatically increases, illustrate as temperature increases (040) crystal face preferential growth.
Fig. 2 is the luminescent spectrum figure of sample under the present embodiment different temperatures, uses Edinburgh, Britain FLS 920 stable state and wink
State luminescence spectrometer measures, and xenon lamp power is 450 watts, and detector is Japan's Hamamatsu refrigeration mode R928P photomultiplier
(operating voltage-1250 volt), data acquisition time of integration is 0.2 second, and scanning step is 1nm.Excitation wavelength is 295nm, by Fig. 2
Understanding, emitting red light under ultraviolet excitation for the sample covers the spectral regions of 550～800, and peak position is 634nm, is Mn2+'s4T1
→6A1Transition.Simultaneously can be best for the luminescent properties of the sample of 1050 DEG C of roastings.
Fig. 3 is the excitation spectrum of sample under the present embodiment different temperatures roasting, and corresponding monitoring wavelength is 634nm；Use
Edinburgh, Britain FLS 920 stable state and transient luminescence spectrophotometer, xenon lamp power is 450 watts, and detector is Japan
Hamamatsu refrigeration mode R928P photomultiplier (operating voltage: 1250 volts), data acquisition time of integration is 0.2 second, scanning
Step-length is 1nm.As it is shown on figure 3, excitation spectrum covers the interval absorption of 250～380nm, show that sample has broadness in ultra-violet (UV) band
Absorb.Peak position is positioned at 295nm and keeps constant.
Embodiment 2
Choose barium monoxide, zinc sulphide and manganous oxide as raw material, according to mol ratio Ba:Zn:S:Mn=1:1:1:0.005
Weigh a certain amount of above-mentioned raw materials respectively, after the ground mixing of raw material, take a part of raw material and add PVA to granulate, take 5g and make
Raw material after Li carries out compressing tablet, takes semi-automatic tablet press machine to keep 3min under 10Mpa, and the cylinder obtaining 25 × 10mm is thin
Piece.Thin slice is placed in corundum boat, roasting 6 hours under 1050 DEG C of vacuum atmospheres；X-ray diffraction analysis shows to which is BaZnOS
Crystalline phase.
By the BaZn after roasting0.995OS:0.5%Mn2+Sample is fixed on sample stage, uses firm with sharp tip
Beautiful rod rubs, and uses fiber spectrometer to collect tribo-luminescence signal simultaneously.Holding friction tips with fibre-optical probe distance is
8mm.Use corundum rod to rub under daylight, be visually observed reddish orange clearly luminous.In darkroom, tribo-luminescence is more
For significantly, and before carrying out tribo-luminescence test, sample does not needs the preexciting of other forms.Fig. 4 is that the friction of sample is sent out
Light spectrum, spectrum covers the red spectral region of 500～700, luminous peak position 585nm.
Embodiment 3
Choose barium hydroxide, zinc sulphide, manganese carbonate as raw material, according to mol ratio Ba:Zn:S:Mn=1:1:1:0.005,
Weigh a certain amount of above-mentioned raw materials.After the ground mixing of raw material, take appropriate in corundum crucible, then crucible be placed in corundum boat,
Corundum boat is pushed in tube furnace, respectively at 1050 DEG C of roastings 5 hours under argon gas atmosphere, naturally cools down with stove, by gained sample
Grind uniformly mechanoluminescence red fluorescence powder BaZn0.995OS:0.5%Mn2+.By gained fluorescent material and transparent epoxy tree
Fat mixes, and cured at room temperature 8h obtains cylindric fluorescent material resin composite materials, a size of 25 × 15mm.Use WEW-
600 type microcomputer control universal testing machines carry out pressure luminous test, and it is 0N～5000N that control applies pressure limit, uses simultaneously
Fiber spectrometer collects pressure luminous signal.
Fig. 5 is luminescent spectrum figure under different size pressure excites for the fluorescent material resin composite materials, luminous as seen from the figure
Intensity strengthens with the increase of pressure applied, and peak position is maintained at～and 610nm is not changed in.By Fig. 6, to luminous intensity with executed
Plus-pressure size carries out linear fit, R2=0.9883, both present good proportional relation.Fig. 7 is the tribo-luminescence of sample, pressure
Power is luminous, the spectrum comparison diagram of luminescence generated by light.
Embodiment 4
Choose barium monoxide, zinc sulphide, manganese dioxide as raw material, by each element mol ratio Ba:Zn:S:Mn=1:1:1:
X, weighs three kinds of raw materials of compound respectively, and totally five groups, proportioning is as follows:
(1) Ba:Zn:S:Mn=1:1:1:0.001, corresponding x=0.10%；
(2) Ba:Zn:S:Mn=1:1:1:0.002, corresponding x=0.20%；
(3) Ba:Zn:S:Mn=1:1:1:0.003, corresponding x=0.30%；
(4) Ba:Zn:S:Mn=1:1:1:0.005, corresponding x=0.50%；
(5) Ba:Zn:S:Mn=1:1:1:0.010, corresponding x=1.00%；
Control mixture total weight is 5g, and 5g mixing raw mill is uniform, puts in corundum crucible, then is placed in crucible
In corundum boat, corundum boat is pushed in tube furnace, in 1050 DEG C of roastings 3 hours under nitrogen atmosphere, naturally cool down with stove,
A series of mechanoluminescence red fluorescence powder BaZn(1-x)OS:xMn2+。
X-ray diffraction analysis shows to which is BaZnOS crystalline phase.The spectral quality of fluorescent material is similar to in embodiment 1.Such as Fig. 8
Shown in, under 295nm excitation wavelength, increase the change of luminous intensity with Mn ion concentration, when x=0.50%, luminescence is the strongest,
The Changing Pattern of the excitation spectrum intensity under 634nm detection simultaneously is consistent with emission spectrum Changing Pattern.
Embodiment 5
Choose brium carbonate, zinc sulphide, manganese oxide as raw material, according to each elemental mole ratios Ba:Zn:S:Mn=1:1:1:
0.005, corresponding x=0.5%；Weighing three kinds of raw materials respectively, control mixture total weight is 5g.After the ground mixing of raw material, put into
In corundum crucible, then crucible is placed in corundum boat, corundum boat is pushed in tube furnace, in 1100 DEG C of roastings 2 under nitrogen atmosphere
Hour, naturally cool down with stove, mechanoluminescence red fluorescence powder BaZn0.995OS:0.5%Mn2+, X-ray diffraction analysis table
Bright which is BaZnOS crystalline phase.The spectral quality of fluorescent material is similar to in embodiment 1.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by described embodiment
Limit, the change made under other any Spirit Essence without departing from the present invention and principle, modifications, replacement, combination, simplification,
All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. a mechanoluminescence red fluorescence powder, it is characterised in that expressing formula is BaZn(1-x)OS:xMn2+, wherein 0.1%≤x
≤ 1.0%, active ions are Mn2+Ion.
2. mechanoluminescence red fluorescence powder according to claim 1, it is characterised in that x=0.5%.
3. the preparation method of a mechanoluminescence red fluorescence powder, it is characterised in that comprise the following steps:
(1) each element mol ratio Ba:Zn:S:Mn=1:1:1:x is pressed；Weigh containing barium compound, sulfur-containing compound respectively, contain zinc
Compound and containing manganese compound as raw material；0.1%≤x≤1.0%；
(2), after the raw materials of compound weighing step (1) grinds uniformly, roasting under protective atmosphere or vacuum, temperature is 900
～1100 DEG C, the time is 2～10 hours；
(3) sample after roasting in step (2) is taken out, grind and i.e. obtain mechanoluminescence red fluorescence powder.
4. the preparation method of mechanoluminescence red fluorescence powder according to claim 3, it is characterised in that described protectiveness gas
Atmosphere is argon gas atmosphere or nitrogen atmosphere.
5. the preparation method of mechanoluminescence red fluorescence powder according to claim 3, it is characterised in that work as x=0.5%
When, it is roasted to 1050 DEG C.
6. the preparation method of mechanoluminescence red fluorescence powder according to claim 3, it is characterised in that described baric chemical combination
Thing is brium carbonate, barium monoxide, the one in barium hydroxide.
7. the preparation method of mechanoluminescence red fluorescence powder according to claim 3, it is characterised in that described sulfur-bearing chemical combination
Thing is zinc sulphide.
8. the preparation method of the mechanoluminescence red fluorescence powder according to claim 3 or 7, it is characterised in that described containing zinc
Compound is zinc sulphide.
9. the preparation method of mechanoluminescence red fluorescence powder according to claim 3, it is characterised in that described containing manganese conjunction
Thing is any one in manganous oxide, manganese oxide, manganese dioxide and manganese carbonate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107739211A (en) * | 2017-11-02 | 2018-02-27 | 杭州显庆科技有限公司 | A kind of yellow green mechanoluminescence ceramic material and preparation method thereof |
| CN114410297A (en) * | 2022-01-24 | 2022-04-29 | 成都大学 | Multi-mode induced red fluorescent material and preparation method thereof |
| CN116254106A (en) * | 2023-03-17 | 2023-06-13 | 中国科学院兰州化学物理研究所 | ZnS-based stress luminescent material and preparation method thereof, and polymer stress luminescent composite material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739211A (en) * | 2017-11-02 | 2018-02-27 | 杭州显庆科技有限公司 | A kind of yellow green mechanoluminescence ceramic material and preparation method thereof |
| CN114410297A (en) * | 2022-01-24 | 2022-04-29 | 成都大学 | Multi-mode induced red fluorescent material and preparation method thereof |
| CN114410297B (en) * | 2022-01-24 | 2023-10-20 | 成都大学 | Multi-mode induced red fluorescent material and preparation method thereof |
| CN116254106A (en) * | 2023-03-17 | 2023-06-13 | 中国科学院兰州化学物理研究所 | ZnS-based stress luminescent material and preparation method thereof, and polymer stress luminescent composite material and preparation method thereof |
| CN116254106B (en) * | 2023-03-17 | 2024-04-12 | 中国科学院兰州化学物理研究所 | ZnS-based stress luminescent material and preparation method thereof, and polymer stress luminescent composite material and preparation method thereof |
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Application publication date: 20161123 |