CN109694710A - A kind of thulium doped, terbium, lithium phosphate magnesium thermoluminescence material of boric acid and preparation method thereof - Google Patents
A kind of thulium doped, terbium, lithium phosphate magnesium thermoluminescence material of boric acid and preparation method thereof Download PDFInfo
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- CN109694710A CN109694710A CN201910017039.7A CN201910017039A CN109694710A CN 109694710 A CN109694710 A CN 109694710A CN 201910017039 A CN201910017039 A CN 201910017039A CN 109694710 A CN109694710 A CN 109694710A
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- boric acid
- lithium phosphate
- terbium
- phosphate magnesium
- thermoluminescence
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- 238000000904 thermoluminescence Methods 0.000 title claims abstract description 88
- 239000000463 material Substances 0.000 title claims abstract description 82
- 229910052775 Thulium Inorganic materials 0.000 title claims abstract description 58
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052771 Terbium Inorganic materials 0.000 title claims abstract description 53
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 title claims abstract description 52
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000004327 boric acid Substances 0.000 title claims abstract description 44
- CUQSVGNVMULJSV-UHFFFAOYSA-K [Li+].[Mg++].[O-]P([O-])([O-])=O Chemical compound [Li+].[Mg++].[O-]P([O-])([O-])=O CUQSVGNVMULJSV-UHFFFAOYSA-K 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 57
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 40
- 239000000126 substance Substances 0.000 claims abstract description 31
- 239000011159 matrix material Substances 0.000 claims abstract description 23
- 238000006467 substitution reaction Methods 0.000 claims abstract description 23
- 150000002500 ions Chemical class 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000000725 suspension Substances 0.000 claims description 52
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 36
- 238000001354 calcination Methods 0.000 claims description 33
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium (III) oxide Inorganic materials [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 claims description 26
- -1 boric acid lithium phosphate magnesium Chemical compound 0.000 claims description 25
- 238000005352 clarification Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 19
- 239000004570 mortar (masonry) Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 3
- 229910019432 Mg(NO3).6H2O Inorganic materials 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 125000003636 chemical group Chemical group 0.000 claims 1
- 238000009837 dry grinding Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 230000005855 radiation Effects 0.000 abstract description 9
- 238000001514 detection method Methods 0.000 abstract description 6
- 231100000331 toxic Toxicity 0.000 abstract description 5
- 230000002588 toxic effect Effects 0.000 abstract description 5
- 229910002651 NO3 Inorganic materials 0.000 description 36
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 18
- 229910015353 LiMgPO4 Inorganic materials 0.000 description 13
- 238000012360 testing method Methods 0.000 description 12
- 239000011777 magnesium Substances 0.000 description 9
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 8
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 8
- 229910052593 corundum Inorganic materials 0.000 description 8
- 239000010431 corundum Substances 0.000 description 8
- 239000011521 glass Substances 0.000 description 8
- ZATZOOLBPDMARD-UHFFFAOYSA-N magnesium;hydrate Chemical compound O.[Mg] ZATZOOLBPDMARD-UHFFFAOYSA-N 0.000 description 8
- 235000019837 monoammonium phosphate Nutrition 0.000 description 8
- 238000007789 sealing Methods 0.000 description 8
- 229910003451 terbium oxide Inorganic materials 0.000 description 8
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 229910015243 LiMg Inorganic materials 0.000 description 6
- 231100000673 dose–response relationship Toxicity 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 238000011896 sensitive detection Methods 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 229910052693 Europium Inorganic materials 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000005457 Black-body radiation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005250 beta ray Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- 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
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7777—Phosphates
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of thulium doped, terbium, the lithium phosphate magnesium thermoluminescence material of boric acid, the chemical composition expression formulas of the thermoluminescence material are as follows: Li Mg1‑x‑yPO4:Tmx,Tby,Bz；Wherein, x is to contain Doped ions Tm3+Substitution matrix in Mg2+Concentration, y be contain Doped ions Tb3+Substitution matrix in Mg2+Concentration, z B3+Concentration, x=y=0.005, z=0.006.The lithium phosphate magnesium thermoluminescence material of thulium doped, terbium provided by the present invention, boric acid, it prepares raw material and preparation method is simple, cost is more cheap, without the raw material that toxic, corrosivity is strong, volatile, it can be applied to the detection that the fields such as medical treatment, environment, nuclear industry carry out dose of radiation, and the performance of product is stable, reproducible, has a good application prospect.
Description
Technical field
The present invention relates to thermoluminescence Material Field, in particular to the lithium phosphate magnesium thermoluminescence of a kind of thulium doped, terbium, boric acid
Material and preparation method thereof.
Background technique
After thermoluminescence refers to that semiconductor or insulating material absorb ionising radiation energy, the phenomenon that by thermoluminescence.Due to
There are certain relationships for the dose of radiation that the thermoluminescence intensity and substance of material are absorbed, and therefore, thermoluminescence material is developed,
And it is widely used in the fields such as radiation protection, environmental monitoring, geological epoch measurement.The thermoluminescent dosemeter generally used now
Material has a LiF:Mg, Ti, LiF:Mg, Gu, P etc., but because the problem of preparation process and material cost, novel thermoluminescence material
Exploitation nevertheless suffer from extensive concern.
Currently, lithium phosphate magnesium light material has LiMgPO4:Tb,Tm、LiMgPO4:Tb,B、 LiMgPO4:Tb、LiMgPO4:
Eu, Sm, B etc. are several, wherein LiMgPO4: the luminous intensity of Tb, Tm material is weaker, LiMgPO4: the Two-Dimensional Heat of Tb, B material are released
Photopeak, peak temperature is lower, and apparent unimodal feature is not presented, and trap is more complicated, should not be used as thermoluminescence material, LiMgPO4:
The two-dimentional thermal glow peak of Tb material, peak temperature is lower, apparent unimodal feature is not presented, trap is more complicated, should not release as heat
Luminescent material, LiMgPO4: Eu, Sm, in 354 DEG C, which is located at after 400 DEG C the thermal glow peak potential temperature of B material,
Signal is interfered vulnerable to black body radiation, is had an impact to the reading of complete dosage, should not be also used as thermoluminescence material.
Summary of the invention
Against the above deficiency, the present invention provides thulium doped one kind, terbium, the lithium phosphate magnesium thermoluminescence material of boric acid and its system
Preparation Method, the thulium doped, terbium, boric acid lithium phosphate magnesium thermoluminescence material can be applied to the fields such as medical treatment, environment, nuclear industry into
The detection of row dose of radiation, prepares raw material and preparation method is simple, and cost is more cheap, and the performance of product is stable, repeats
Property is good.
To achieve the above object, first aspect present invention provides:
The lithium phosphate magnesium thermoluminescence material of a kind of thulium doped, terbium, boric acid, the chemical composition expression formula of the thermoluminescence material
Are as follows: LiMg1-x-yPO4:Tmx,Tby,Bz；Wherein, x is to contain Doped ions Tm3+Substitution matrix in Mg2+Concentration, y be containing
There is Doped ions Tb3+Substitution matrix in Mg2+Concentration, z B3+Concentration, 0.003≤x≤0.03,0.003≤y≤
0.03,0.003≤z≤0.05.
Preferably, 0.003≤x≤0.01,0.003≤y≤0.01,0.005≤z≤0.03.
It is further preferred that x=y=0.005, z=0.006.
The lithium phosphate magnesium thermoluminescence material of above-mentioned thulium doped, terbium, boric acid, matrix are phosphate LiMgPO4, shine
Center is trivalent rare earth thulium ion Tm3+.The Tb being co-doped with3+Play the role of energy transfer in the material, boric acid is mended as charge
Repay the luminescence enhancement that agent makes sample.Sample is after receiving doses, the transition by way of thermal excitation, launch wavelength model
It encloses for 445-505 nm, it is typical Tm that strongest emission peak, which is located at 455nm,3+Transition transmitting, emission peak potential temperature is in 323
℃.The thermal glow peak peak temperature is higher, and peak shape is single, better heat stability, and the launch wavelength of signal is located at thermoluminescence three-dimensional spectrum
Blue end, coincide with the maximum sensitive volume of most of photomultiplier tube.
Second aspect of the present invention provide above-described thulium doped, terbium, boric acid lithium phosphate magnesium thermoluminescence material preparation
Method, the preparation method include the following steps:
Step 1: pressing chemical composition expression formula LiMg1-x-yPO4:Tmx,Tby,BzIn each chemical composition stoichiometric ratio,
The following raw material for standby of corrresponding quality ratio is weighed respectively:
A component: Tb4O7、Tm2O3；B component: LiNO3、Mg(NO3).6H2O、NH4HPO4、 H3BO3；
Step 2: a component is configured to Tb (NO3)3、Tm(NO3)3B component is added to 10-15mL deionized water by solution
In, it stirs evenly, makes solution in suspension；
Step 3: pipetting Tb (NO3)3、Tm(NO3)3Solution stirs 10-30 minutes at 80-100 DEG C into suspension,
Until solution is rendered as clarification suspension；
Step 4: clarification suspension is heated 3-7 hours at 100-150 DEG C, solvent is evaporated, obtains being evaporated object, it
After will be evaporated object grinding uniformly, be allowed to obtain mixture, which is roasted in air atmosphere in powdered, roasting temperature
Degree is 850-1050 DEG C, and calcining time is 2-6 hours, and calcining matter is obtained after roasting, calcining matter is cooled to room temperature, obtains sample
Product；
Step 5: sample being ground uniformly, the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium, boric acid is obtained.
Preferably, in step 4, stirring operation is specifically that magneton is added in suspension, and suspension is placed on magnetic later
It is stirred on power blender.
Preferably, in step 3, the time of suspension stirring is 15-25 minutes, in step 4, by clarification suspension heating
The time being evaporated is 4-6 hours, and heating rate when mixture roasts is 3-5 DEG C/s, and calcining time is 4-6 hours.
It is further preferred that the time of suspension stirring is 20 minutes, in step 4 in step 3, clarification suspension is added
The time that heat is evaporated is 5 hours, and heating rate when mixture roasts is 5 DEG C/s, and calcining time is 4 hours.
Preferably, in step 4, mixture is in horizontal tube kiln roasting.
Preferably, in step 5, sample is placed in mortar and is fully ground.
Preferably, step 5 is encapsulated preservation after obtaining the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium, boric acid.
The beneficial effects of the present invention are:
1, it prepares that raw material is simple, safety, strong corrosive, toxic, volatile raw material is not used, and preparation method is simple, at
This is lower, and powder sample preferably shows the characteristic of thermoluminescence material；
2, product, which is located at 323 DEG C or so, a single glow peak, and signal is not easy to fail at normal temperature, after tested, sample
The thermoluminescence signal of product fails 8.43% in 34 days, in 30 test periods, standard error 4.6%, and stability
Preferably, repeatability is high；
3, the launch wavelength of product glow peak is 455nm, is the characteristic emission of rare earth thulium ion, which is located at blue light
Wave band better conforms to the investigative range in photomultiplier tube maximum sensitive detection area；
4, the dose response curve of product is shown, is had preferable linear characteristic in 0.08-2000Gy, is conducive to low dosage
With the radiation detection of high dose.
Detailed description of the invention
Fig. 1 is the influence schematic diagram of different boric acid doping concentrations and different firing temperatures to sample thermoluminescence intensity；
Fig. 2 is LiMg of the invention0.99PO4:Tm0.005,Tb0.005,B0.006The thermoluminescence three-dimensional spectrogram of phosphor；
Fig. 3 is LiMg of the invention0.99PO4:Tm0.005,Tb0.005,B0.006The repetition measurement data record of phosphor
Figure；
Fig. 4 is LiMg of the invention0.99PO4:Tm0.005,Tb0.005,B0.006The fall time tendency chart of phosphor；
Fig. 5 is LiMg of the invention0.99PO4:Tm0.005,Tb0.005,B0.006The dose response curve schematic diagram of phosphor；
Fig. 6 is LiMg of the invention0.99PO4:Tm0.005,Tb0.005,B0.006Phosphor and business LiF:Mg, Gu, P's
Thermoluminescence intensity comparison diagram；
Fig. 7 is LiMg of the invention0.99PO4:Tm0.005,Tb0.005,B0.006Phosphor and LiMgPO4:Tm0.005,Tb0.005
The normalization thermoluminescence intensity comparison diagram of phosphor.
Specific embodiment
For that can further appreciate that the contents of the present invention, feature and effect, following embodiment of hereby illustrating, and cooperate attached drawing detailed
Carefully it is described as follows.It should be noted that following embodiment be it is descriptive, be not restrictive, cannot thus limit the present invention
Protection scope.
Reagent of the present invention, equipment are the conventional reagent of the art, equipment.Unless otherwise specified, implement
Reagent used in example is commercially available with material.
Embodiment 1
The lithium phosphate magnesium thermoluminescence material of a kind of thulium doped, terbium, boric acid, the chemical composition expression formula of the thermoluminescence material
Are as follows: LiMg1-x-yPO4:Tmx,Tby,Bz；Wherein, x is to contain Doped ions Tm3+Substitution matrix in Mg2+Concentration, y be containing
There is Doped ions Tb3+Substitution matrix in Mg2+Concentration, z B3+Concentration, x=y=0.005, z=0.006.
Above-mentioned thulium doped, terbium, boric acid lithium phosphate magnesium thermoluminescence material preparation method, include the following steps:
Step 1: pressing chemical composition expression formula LiMg1-x-yPO4:Tmx,Tby,BzIn each chemical composition stoichiometric ratio,
The following raw material for standby of corrresponding quality ratio is weighed respectively:
A component: Tb4O7(terbium oxide, 99.99%), Tm2O3(thulium oxide, 99.99%)；B component: LiNO3(lithium nitrate,
Analyze pure), Mg (NO3).6H2O (nitric hydrate magnesium is analyzed pure), NH4HPO4、H3BO3(ammonium dihydrogen phosphate is analyzed pure)；
Step 2: a component is configured to Tb (NO3)3、Tm(NO3)3B component is added in beaker by solution, and past beaker
Middle addition 10-15mL deionized water, is stirred evenly with glass bar, makes solution in suspension；
Step 3: pipetting Tb (NO with liquid-transfering gun3)3、Tm(NO3)3Solution stirs 10- at 80-100 DEG C into suspension
30 minutes, until solution is rendered as clarification suspension；
Step 4: clarification suspension is placed on electric furnace, is heated 4-6 hours at 100-150 DEG C, is evaporated solvent,
It obtains being evaporated object, object will be evaporated later be placed in mortar and grind uniformly, and be allowed to obtain mixture in powdered, mixture is turned
It after moving to corundum crucible, is placed in horizontal pipe furnace, is roasted in air atmosphere, maturing temperature is 950 DEG C, and calcining time is
2-6 hours, heating rate when roasting was 3-5 DEG C/s, obtains calcining matter after roasting, calcining matter is cooled to room temperature, obtain
Sample；
Step 5: taking out sample, sample is placed in mortar and is ground uniformly, the lithium phosphate magnesium of thulium doped, terbium, boric acid is obtained
Thermoluminescence material, finally, tube sealing saves.
Embodiment 2
The lithium phosphate magnesium thermoluminescence material of a kind of thulium doped, terbium, boric acid, the chemical composition expression formula of the thermoluminescence material
Are as follows: LiMg1-x-yPO4:Tmx,Tby,Bz；Wherein, x is to contain Doped ions Tm3+Substitution matrix in Mg2+Concentration, y be containing
There is Doped ions Tb3+Substitution matrix in Mg2+Concentration, z B3+Concentration, x=y=0.005, z=0.006.
Above-mentioned thulium doped, terbium, boric acid lithium phosphate magnesium thermoluminescence material preparation method, include the following steps:
Step 1: pressing chemical composition expression formula LiMg1-x-yPO4:Tmx,Tby,BzIn each chemical composition stoichiometric ratio,
The following raw material for standby of corrresponding quality ratio is weighed respectively:
A component: Tb4O7(terbium oxide, 99.99%), Tm2O3(thulium oxide, 99.99%)；B component: LiNO3(lithium nitrate,
Analyze pure), Mg (NO3).6H2O (nitric hydrate magnesium is analyzed pure), NH4HPO4、H3BO3(ammonium dihydrogen phosphate is analyzed pure)；
Step 2: a component is configured to Tb (NO3)3、Tm(NO3)3B component is added in beaker by solution, and past beaker
Middle addition 10-15mL deionized water, is stirred evenly with glass bar, makes solution in suspension；
Step 3: pipetting Tb (NO with liquid-transfering gun3)3、Tm(NO3)3Solution stirs 10- at 80-100 DEG C into suspension
30 minutes, until solution is rendered as clarification suspension；
Step 4: clarification suspension is placed on electric furnace, is heated 3-7 hours at 100-150 DEG C, is evaporated solvent,
It obtains being evaporated object, object will be evaporated later be placed in mortar and grind uniformly, and be allowed to obtain mixture in powdered, mixture is turned
It after moving to corundum crucible, is placed in horizontal pipe furnace, is roasted in air atmosphere, maturing temperature is 800 DEG C, and calcining time is
2-6 hours, heating rate when roasting was 3-5 DEG C/s, obtains calcining matter after roasting, calcining matter is cooled to room temperature, obtain
Sample；
Step 5: taking out sample, sample is placed in mortar and is ground uniformly, the lithium phosphate magnesium of thulium doped, terbium, boric acid is obtained
Thermoluminescence material, finally, tube sealing saves.
Embodiment 3
The lithium phosphate magnesium thermoluminescence material of a kind of thulium doped, terbium, boric acid, the chemical composition expression formula of the thermoluminescence material
Are as follows: LiMg1-x-yPO4:Tmx,Tby,Bz；Wherein, x is to contain Doped ions Tm3+Substitution matrix in Mg2+Concentration, y be containing
There is Doped ions Tb3+Substitution matrix in Mg2+Concentration, z B3+Concentration, x=y=0.005, z=0.006.
Above-mentioned thulium doped, terbium, boric acid lithium phosphate magnesium thermoluminescence material preparation method, include the following steps:
Step 1: pressing chemical composition expression formula LiMg1-x-yPO4:Tmx,Tby,BzIn each chemical composition stoichiometric ratio,
The following raw material for standby of corrresponding quality ratio is weighed respectively:
A component: Tb4O7(terbium oxide, 99.99%), Tm2O3(thulium oxide, 99.99%)；B component: LiNO3(lithium nitrate,
Analyze pure), Mg (NO3).6H2O (nitric hydrate magnesium is analyzed pure), NH4HPO4、H3BO3(ammonium dihydrogen phosphate is analyzed pure)；
Step 2: a component is configured to Tb (NO3)3、Tm(NO3)3B component is added in beaker by solution, and past beaker
Middle addition 10-15mL deionized water, is stirred evenly with glass bar, makes solution in suspension；
Step 3: pipetting Tb (NO with liquid-transfering gun3)3、Tm(NO3)3Solution stirs 10- at 80-100 DEG C into suspension
30 minutes, until solution is rendered as clarification suspension；
Step 4: clarification suspension is placed on electric furnace, is heated 3-7 hours at 100-150 DEG C, is evaporated solvent,
It obtains being evaporated object, object will be evaporated later be placed in mortar and grind uniformly, and be allowed to obtain mixture in powdered, mixture is turned
It after moving to corundum crucible, is placed in horizontal pipe furnace, is roasted in air atmosphere, maturing temperature is 850 DEG C, and calcining time is
2-6 hours, heating rate when roasting was 3-5 DEG C/s, obtains calcining matter after roasting, calcining matter is cooled to room temperature, obtain
Sample；
Step 5: taking out sample, sample is placed in mortar and is ground uniformly, the lithium phosphate magnesium of thulium doped, terbium, boric acid is obtained
Thermoluminescence material, finally, tube sealing saves.
Embodiment 4
The lithium phosphate magnesium thermoluminescence material of a kind of thulium doped, terbium, boric acid, the chemical composition expression formula of the thermoluminescence material
Are as follows: LiMg1-x-yPO4:Tmx,Tby,Bz；Wherein, x is to contain Doped ions Tm3+Substitution matrix in Mg2+Concentration, y be containing
There is Doped ions Tb3+Substitution matrix in Mg2+Concentration, z B3+Concentration, x=y=0.005, z=0.006.
Above-mentioned thulium doped, terbium, boric acid lithium phosphate magnesium thermoluminescence material preparation method, include the following steps:
Step 1: pressing chemical composition expression formula LiMg1-x-yPO4:Tmx,Tby,BzIn each chemical composition stoichiometric ratio,
The following raw material for standby of corrresponding quality ratio is weighed respectively:
A component: Tb4O7(terbium oxide, 99.99%), Tm2O3(thulium oxide, 99.99%)；B component: LiNO3(lithium nitrate,
Analyze pure), Mg (NO3).6H2O (nitric hydrate magnesium is analyzed pure), NH4HPO4、H3BO3(ammonium dihydrogen phosphate is analyzed pure)；
Step 2: a component is configured to Tb (NO3)3、Tm(NO3)3B component is added in beaker by solution, and past beaker
Middle addition 10-15mL deionized water, is stirred evenly with glass bar, makes solution in suspension；
Step 3: pipetting Tb (NO with liquid-transfering gun3)3、Tm(NO3)3Solution stirs 10- at 80-100 DEG C into suspension
30 minutes, until solution is rendered as clarification suspension；
Step 4: clarification suspension is placed on electric furnace, is heated 3-7 hours at 100-150 DEG C, is evaporated solvent,
It obtains being evaporated object, object will be evaporated later be placed in mortar and grind uniformly, and be allowed to obtain mixture in powdered, mixture is turned
It after moving to corundum crucible, is placed in horizontal pipe furnace, is roasted in air atmosphere, maturing temperature is 900 DEG C, and calcining time is
2-6 hours, heating rate when roasting was 3-5 DEG C/s, obtains calcining matter after roasting, calcining matter is cooled to room temperature, obtain
Sample；
Step 5: taking out sample, sample is placed in mortar and is ground uniformly, the lithium phosphate magnesium of thulium doped, terbium, boric acid is obtained
Thermoluminescence material, finally, tube sealing saves.
Embodiment 5
The lithium phosphate magnesium thermoluminescence material of a kind of thulium doped, terbium, boric acid, the chemical composition expression formula of the thermoluminescence material
Are as follows: LiMg1-x-yPO4:Tmx,Tby,Bz；Wherein, x is to contain Doped ions Tm3+Substitution matrix in Mg2+Concentration, y be containing
There is Doped ions Tb3+Substitution matrix in Mg2+Concentration, z B3+Concentration, x=y=0.005, z=0.006.
Above-mentioned thulium doped, terbium, boric acid lithium phosphate magnesium thermoluminescence material preparation method, include the following steps:
Step 1: pressing chemical composition expression formula LiMg1-x-yPO4:Tmx,Tby,BzIn each chemical composition stoichiometric ratio,
The following raw material for standby of corrresponding quality ratio is weighed respectively:
A component: Tb4O7(terbium oxide, 99.99%), Tm2O3(thulium oxide, 99.99%)；B component: LiNO3(lithium nitrate,
Analyze pure), Mg (NO3).6H2O (nitric hydrate magnesium is analyzed pure), NH4HPO4、H3BO3(ammonium dihydrogen phosphate is analyzed pure)；
Step 2: a component is configured to Tb (NO3)3、Tm(NO3)3B component is added in beaker by solution, and past beaker
Middle addition 10-15mL deionized water, is stirred evenly with glass bar, makes solution in suspension；
Step 3: pipetting Tb (NO with liquid-transfering gun3)3、Tm(NO3)3Solution stirs 10- at 80-100 DEG C into suspension
30 minutes, until solution is rendered as clarification suspension；
Step 4: clarification suspension is placed on electric furnace, is heated 3-7 hours at 100-150 DEG C, is evaporated solvent,
It obtains being evaporated object, object will be evaporated later be placed in mortar and grind uniformly, and be allowed to obtain mixture in powdered, mixture is turned
It after moving to corundum crucible, is placed in horizontal pipe furnace, is roasted in air atmosphere, maturing temperature is 1000 DEG C, and calcining time is
2-6 hours, heating rate when roasting was 3-5 DEG C/s, obtains calcining matter after roasting, calcining matter is cooled to room temperature, obtain
Sample；
Step 5: taking out sample, sample is placed in mortar and is ground uniformly, the lithium phosphate magnesium of thulium doped, terbium, boric acid is obtained
Thermoluminescence material, finally, tube sealing saves.
Embodiment 6
The lithium phosphate magnesium thermoluminescence material of a kind of thulium doped, terbium, boric acid, the chemical composition expression formula of the thermoluminescence material
Are as follows: LiMg1-x-yPO4:Tmx,Tby,Bz；Wherein, x is to contain Doped ions Tm3+Substitution matrix in Mg2+Concentration, y be containing
There is Doped ions Tb3+Substitution matrix in Mg2+Concentration, z B3+Concentration, x=y=0.005, z=0.006.
Above-mentioned thulium doped, terbium, boric acid lithium phosphate magnesium thermoluminescence material preparation method, include the following steps:
Step 1: pressing chemical composition expression formula LiMg1-x-yPO4:Tmx,Tby,BzIn each chemical composition stoichiometric ratio,
The following raw material for standby of corrresponding quality ratio is weighed respectively:
A component: Tb4O7(terbium oxide, 99.99%), Tm2O3(thulium oxide, 99.99%)；B component: LiNO3(lithium nitrate,
Analyze pure), Mg (NO3).6H2O (nitric hydrate magnesium is analyzed pure), NH4HPO4、H3BO3(ammonium dihydrogen phosphate is analyzed pure)；
Step 2: a component is configured to Tb (NO3)3、Tm(NO3)3B component is added in beaker by solution, and past beaker
Middle addition 10-15mL deionized water, is stirred evenly with glass bar, makes solution in suspension；
Step 3: pipetting Tb (NO with liquid-transfering gun3)3、Tm(NO3)3Solution stirs 10- at 80-100 DEG C into suspension
30 minutes, until solution is rendered as clarification suspension；
Step 4: clarification suspension is placed on electric furnace, is heated 3-7 hours at 100-150 DEG C, is evaporated solvent,
It obtains being evaporated object, object will be evaporated later be placed in mortar and grind uniformly, and be allowed to obtain mixture in powdered, mixture is turned
It after moving to corundum crucible, is placed in horizontal pipe furnace, is roasted in air atmosphere, maturing temperature is 1050 DEG C, and calcining time is
2-6 hours, heating rate when roasting was 3-5 DEG C/s, obtains calcining matter after roasting, calcining matter is cooled to room temperature, obtain
Sample；
Step 5: taking out sample, sample is placed in mortar and is ground uniformly, the lithium phosphate magnesium of thulium doped, terbium, boric acid is obtained
Thermoluminescence material, finally, tube sealing saves.
Control group
The lithium phosphate magnesium thermoluminescence material of a kind of thulium doped, terbium, boric acid, other feature is same as Example 1, difference
Be in and take 0,0.003,0.01,0.03,0.05 respectively in: the concentration y of boric acid, mixture roasted respectively by room temperature to 800 DEG C,
850 DEG C, 900 DEG C, 950 DEG C, 1000 DEG C, 1050 DEG C, obtain 30 groups of different control samples.
Examples 1 to 6 and control group experiment are compared, referring to Fig.1, Fig. 1 is the boric acid and difference of different levels of doping
Firing temperature influences schematic diagram to the thermoluminescence luminous intensity of sample, it can be found that: when firing temperature is 950 DEG C, boric acid concentration
When being 0.6%, luminous intensity highest.
Referring further to Figure 2, Fig. 2 is embodiment 1LiMg0.99PO4:Tm0.005,Tb0.005,B0.006The thermoluminescence of phosphor
Three-dimensional spectrogram, it can be obtained from the figure that going out: LiMg0.99PO4:Tm0.005,Tb0.005,B0.006The launch wavelength range of phosphor is 445-
505nm, strongest emission peak are located at 455nm, are typical Tm3+Transition transmitting.The wavelength is located at blue wave band, preferably
Meet the investigative range in photomultiplier tube maximum sensitive detection area, emission peak potential temperature is in 323 DEG C.
Embodiment 7
The lithium phosphate magnesium thermoluminescence material of a kind of thulium doped, terbium, boric acid, the chemical composition expression formula of the thermoluminescence material
Are as follows: LiMg1-x-yPO4:Tmx,Tby,Bz；Wherein, x is to contain Doped ions Tm3+Substitution matrix in Mg2+Concentration, y be containing
There is Doped ions Tb3+Substitution matrix in Mg2+Concentration, z B3+Concentration, 0.003≤x≤0.03,0.003≤y≤
0.03,0.003≤z≤0.05.
Above-mentioned thulium doped, terbium, boric acid lithium phosphate magnesium thermoluminescence material preparation method, include the following steps:
Step 1: pressing chemical composition expression formula LiMg1-x-yPO4:Tmx,Tby,BzIn each chemical composition stoichiometric ratio,
The following raw material for standby of corrresponding quality ratio is weighed respectively:
A component: Tb4O7(terbium oxide, 99.99%), Tm2O3(thulium oxide, 99.99%)；B component: LiNO3(lithium nitrate,
Analyze pure), Mg (NO3).6H2O (nitric hydrate magnesium is analyzed pure), NH4HPO4、H3BO3(ammonium dihydrogen phosphate is analyzed pure)；
Step 2: a component is configured to Tb (NO3)3、Tm(NO3)3B component is added in beaker by solution, and past beaker
Middle addition 10-15mL deionized water, is stirred evenly with glass bar, makes solution in suspension；
Step 3: pipetting Tb (NO with liquid-transfering gun3)3、Tm(NO3)3Solution stirs 15- at 80-100 DEG C into suspension
25 minutes, until solution is rendered as clarification suspension；
Step 4: clarification suspension is placed on electric furnace, is heated 4-6 hours at 100-150 DEG C, is evaporated solvent,
It obtains being evaporated object, object will be evaporated later be placed in mortar and grind uniformly, and be allowed to obtain mixture in powdered, mixture is turned
It after moving to corundum crucible, is placed in horizontal pipe furnace, is roasted in air atmosphere, maturing temperature is 850-1050 DEG C, when roasting
Between be 4-6 hour, mixture roast when heating rate be 3-5 DEG C/s, obtain calcining matter after roasting, calcining matter be cooled to
Room temperature obtains sample；
Step 5: taking out sample, sample is placed in mortar and is ground uniformly, the lithium phosphate magnesium of thulium doped, terbium, boric acid is obtained
Thermoluminescence material, finally, tube sealing saves.
Thulium doped provided by the present embodiment, terbium, boric acid lithium phosphate magnesium thermoluminescence material prepare that raw material is simple, safety,
Strong corrosive, toxic, volatile raw material is not used, and preparation method is simple, cost is relatively low, and powder sample is preferably presented
The characteristic of thermoluminescence material out, product, which is located at 323 DEG C, a single glow peak, and signal is not easy to fail at normal temperature, through surveying
Examination, the thermoluminescence signal of sample fail 8.43% in 34 days, in 30 test periods, standard error 4.6%,
Stability is preferable, repeatability is high, and it is the characteristic emission of rare earth thulium ion, the wave that the launch wavelength of product glow peak, which is 455nm,
It is long to be located at blue wave band, the investigative range in photomultiplier tube maximum sensitive detection area is better conformed to, the dose response of product is bent
Line shows there is preferable linear characteristic in 0.08-2000Gy, is conducive to the radiation detection of low dosage and high dose.
Embodiment 8
The lithium phosphate magnesium thermoluminescence material of a kind of thulium doped, terbium, boric acid, the chemical composition expression formula of the thermoluminescence material
Are as follows: LiMg1-x-yPO4:Tmx,Tby,Bz；Wherein, x is to contain Doped ions Tm3+Substitution matrix in Mg2+Concentration, y be containing
There is Doped ions Tb3+Substitution matrix in Mg2+Concentration, z B3+Concentration, 0.003≤x≤0.01,0.003≤y≤
0.01,0.005 ≤z≤0.03。
Above-mentioned thulium doped, terbium, boric acid lithium phosphate magnesium thermoluminescence material preparation method, include the following steps:
Step 1: pressing chemical composition expression formula LiMg1-x-yPO4:Tmx,Tby,BzIn each chemical composition stoichiometric ratio,
The following raw material for standby of corrresponding quality ratio is weighed respectively:
A component: LiNO3(lithium nitrate is analyzed pure), Tb4O7(terbium oxide, 99.99%), Tm2O3(thulium oxide,
99.99%)；B component: Mg (NO3).6H2O (nitric hydrate magnesium is analyzed pure), NH4HPO4、H3BO3(ammonium dihydrogen phosphate, analysis
It is pure)；
Step 2: a component is configured to Tb (NO3)3、Tm(NO3)3B component is added in beaker by solution, and past beaker
Middle addition 10-15mL deionized water, is stirred evenly with glass bar, makes solution in suspension；
Step 3: pipetting Tb (NO with liquid-transfering gun3)3、Tm(NO3)3Solution stirs 20 at 80-100 DEG C into suspension
Minute, until solution is rendered as clarification suspension；
Step 4: clarification suspension being placed on electric furnace and is heated 5 hours, solvent is evaporated, obtains being evaporated object, later will
It is evaporated object and is placed in mortar and grind uniformly, be allowed to obtain mixture, after mixture is transferred to corundum crucible, set in powdered
In horizontal pipe furnace, roasted in air atmosphere, maturing temperature be 950 DEG C, mixture roast when heating rate be 5 DEG C/
S, calcining time are 4 hours, and calcining matter is obtained after roasting, calcining matter is cooled to room temperature, obtains sample；
Step 5: taking out sample, sample is placed in mortar and is ground uniformly, the lithium phosphate magnesium of thulium doped, terbium, boric acid is obtained
Thermoluminescence material, finally, tube sealing saves.
Thulium doped provided by the present embodiment, terbium, boric acid lithium phosphate magnesium thermoluminescence material prepare that raw material is simple, safety,
Strong corrosive, toxic, volatile raw material is not used, and preparation method is simple, cost is relatively low, and powder sample is preferably presented
The characteristic of thermoluminescence material out, product, which is located at 323 DEG C, a single glow peak, and signal is not easy to fail at normal temperature, through surveying
Examination, the thermoluminescence signal of sample fail 8.43% in 34 days, in 30 test periods, standard error 4.6%,
Stability is preferable, repeatability is high, and it is the characteristic emission of rare earth thulium ion, the wave that the launch wavelength of product glow peak, which is 455nm,
It is long to be located at blue wave band, the investigative range in photomultiplier tube maximum sensitive detection area is better conformed to, the dose response of product is bent
Line shows there is preferable linear characteristic in 0.08-2000Gy, is conducive to the radiation detection of low dosage and high dose.
Embodiment 9LiMg0.99PO4:Tm0.005,Tb0.005,B0.006The reperformance test of phosphor
Weigh a certain amount of embodiment 1LiMg0.99PO4:Tm0.005,Tb0.005,B0.006Phosphor sample, in identical spoke
According under the test conditions such as dosage, heating rate, with step 1: annealing, step 2: irradiation doses, step 3: testing is one
Experimental period, follow-on test 30 times.Data are obtained to be counted: as shown in figure 3, in 30 test periods, standard error
It is 4.6%, it was demonstrated that repeatability is good.
Embodiment 10LiMg0.99PO4:Tm0.005,Tb0.005,B0.006The fall time measurement experiment of phosphor
Weigh equivalent embodiment 1LiMg0.99PO4:Tm0.005,Tb0.005,B0.0068 parts of phosphor sample, in identical test
Under the conditions of irradiate doses, be placed in Low background vitriol chamber (darkroom) and be placed and held in the temperature of room temperature.Respectively at the 0th day
(can measure) takes out for the 1st day, the 2nd day, the 3rd day, the 8th day, the 12nd day, the 16th day, the 25th day, the 34th day, and measurement heat is released
Light curve, test condition are consistent.The luminous intensity of the high temperature glow peak of test curve is subjected to integral and obtains respective strengths
Value will obtain data and count: as shown in figure 4, the thermoluminescence signal of sample fails 8.43% in 34 days, it was demonstrated that stablize
Property is preferable.
Embodiment 11LiMg0.99PO4:Tm0.005,Tb0.005,B0.006The dose response of phosphor is tested
By embodiment 1LiMg0.99PO4:Tm0.005,Tb0.005,B0.006Phosphor sample irradiates 0.08-10000Gy's respectively
After β ray, Thermo-luminescence is obtained under identical testing conditions, and the luminous intensity of high temperature glow peak is subjected to integral and is obtained
Respective strengths value is obtained, the data of acquisition are counted, as shown in figure 5, sample has preferably within the scope of 0.08-2000Gy
It is linear.
Comparative example 1
By LiMg0.99PO4:Tm0.005,Tb0.005,B0.006Phosphor is compared with business LiF:Mg, Gu, P, takes quality
Identical two sample, at identical conditions after β x ray irradiation x 0.08Gy, with the rate of 5 DEG C/s by room temperature to 500
DEG C, as shown in fig. 6, obtaining the Thermo-luminescence comparison diagram of the two, as seen from the figure, LiMg0.99PO4:Tm0.005,Tb0.005,B0.006
Glow peak temperature compared with LiF:Mg, Gu, P high, 0.93 times of (comparing peak value)/3.4 times (ratio of luminous intensity LiF:Mg, Gu, P
Compared with integrated intensity).
Comparative example 2
By LiMg0.99PO4:Tm0.005,Tb0.005,B0.006Phosphor and LiMgPO4:Tm0.005,Tb0.005Phosphor is opposed
Than two samples identical in quality being taken, at identical conditions after β x ray irradiation x 0.08Gy, with the rate of 5 DEG C/s by room temperature
500 DEG C are warming up to, the Thermo-luminescence comparison diagram of the two is obtained, as shown in fig. 7, as seen from the figure, LiMg0.99PO4:Tm0.005,
Tb0.005,B0.006Glow peak temperature compared with LiMgPO4:Tm0.005,Tb0.005Height, luminous intensity LiMgPO4:Tm0.005,Tb0.005's
1.82 times of (comparing peak value)/1.75 times (comparing integrated intensity).
To sum up, the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium provided by the present invention, boric acid, prepares raw material and system
Preparation Method is simple, and cost is more cheap, without the raw material that toxic, corrosivity is strong, volatile, can be applied to medical treatment, environment, core
The fields such as industry carry out the detection of dose of radiation, and the performance of product is stable, reproducible, has a good application prospect.
The above, preferable specific embodiment only of the invention, but protection scope of the present invention is not limited to
This, anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention
And its design is subject to equivalent substitution or change, should be covered by the scope of protection of the present invention.
Claims (10)
1. the lithium phosphate magnesium thermoluminescence material of a kind of thulium doped, terbium, boric acid, which is characterized in that the chemical group of the thermoluminescence material
At expression formula are as follows: LiMg1-x-yPO4:Tmx,Tby,Bz；Wherein, x is to contain Doped ions Tm3+Substitution matrix in Mg2+It is dense
Degree, y are to contain Doped ions Tb3+Substitution matrix in Mg2+Concentration, z B3+Concentration, 0.003≤x≤0.03,0.003
≤ y≤0.03,0.003≤z≤0.05.
2. the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium according to claim 1, boric acid, which is characterized in that 0.003
≤ x≤0.01,0.003≤y≤0.01,0.005≤z≤0.03.
3. the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium according to claim 2, boric acid, which is characterized in that x=y=
0.005, z=0.006.
4. according to claim 1~3 described in any item thulium doped, terbiums, boric acid lithium phosphate magnesium thermoluminescence material preparation side
Method, which comprises the steps of:
Step 1: pressing chemical composition expression formula LiMg1-x-yPO4:Tmx,Tby,BzIn each chemical composition stoichiometric ratio, claim respectively
Take the following raw material for standby of corrresponding quality ratio:
A component: Tb4O7、Tm2O3；B component: LiNO3、Mg(NO3).6H2O、NH4HPO4、H3BO3；
Step 2: a component is configured to Tb (NO3)3、Tm(NO3)3B component is added in 10-15mL deionized water, stirs by solution
It mixes uniformly, makes solution in suspension；
Step 3: pipetting Tb (NO3)3、Tm(NO3)3Solution stirs 10-30 minutes at 80-100 DEG C into suspension, until molten
Liquid is rendered as clarification suspension；
Step 4: clarification suspension being heated 3-7 hours at 100-150 DEG C, solvent is evaporated, obtains being evaporated object, will be steamed later
Dry grinding uniformly, is allowed to be in powdered, obtains mixture, which is roasted in air atmosphere, maturing temperature is
850-1050 DEG C, calcining time is 2-6 hours, and calcining matter is obtained after roasting, calcining matter is cooled to room temperature, obtains sample；
Step 5: sample being ground uniformly, the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium, boric acid is obtained.
5. the preparation method of the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium according to claim 4, boric acid, feature
It is, in step 4, stirring operation is specifically that magneton is added in suspension, and suspension is placed on magnetic stirring apparatus later
Stirring.
6. the preparation method of the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium according to claim 4, boric acid, feature
It is, in step 3, the time of suspension stirring is 15-25 minute, in step 4, will clarify suspension and heat time for being evaporated and be
4-6 hours, heating rate when mixture roasts was 3-5 DEG C/s, and calcining time is 4-6 hours.
7. the preparation method of the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium according to claim 6, boric acid, feature
It is, in step 3, the time of suspension stirring is 20 minutes, in step 4, and will clarify the time that suspension heating is evaporated is 5 small
When, heating rate when mixture roasts is 5 DEG C/s, and calcining time is 4 hours.
8. the preparation method of the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium according to claim 4, boric acid, feature
It is, in step 4, mixture is in horizontal tube kiln roasting.
9. the preparation method of the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium according to claim 4, boric acid, feature
It is, in step 5, sample is placed in mortar and is fully ground.
10. the preparation method of the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium according to claim 4, boric acid, feature
It is, step 5 is encapsulated preservation after obtaining the lithium phosphate magnesium thermoluminescence material of thulium doped, terbium, boric acid.
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| RU2821465C1 (en) * | 2024-01-31 | 2024-06-24 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Optical matrix for thermoluminescent material |
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