CN108426651B - The temp measuring method for carrying out anti-white LED light source interference using purple light is converted on thulium ion - Google Patents
The temp measuring method for carrying out anti-white LED light source interference using purple light is converted on thulium ion Download PDFInfo
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- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
- G01K11/006—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using measurement of the effect of a material on microwaves or longer electromagnetic waves, e.g. measuring temperature via microwaves emitted by the object
Abstract
The temp measuring method for carrying out anti-white LED light source interference using purple light is converted on thulium ion, the present invention relates to a kind of temp measuring methods for carrying out anti-white LED light source interference using purple light is converted on thulium ion.The problem of will receive the interference of common white LED light source the purpose of the present invention is to solve existing thermometry, method are as follows: the exciting light that excitaton source issues is to Yb3+And Tm3+The nanocrystal NaYF of ion doping4It is excited, monitors two fluorescent belts that central wavelength under different temperatures is located at 290nm and 345nm, integrated, and make functional relation, sample is placed in environment to be measured, obtains the intensity rate of two fluorescent belts, be updated in function up to temperature value.The present invention is able to carry out the temperature measurement of anti-white LED light source interference, to obtain more accurate result.The present invention is applied to rare-earth fluorescent field of temperature measurement.
Description
Technical field
It the present invention relates to the use of and convert the temp measuring method that purple light carries out anti-white LED light source interference on thulium ion.
Background technique
Temperature is a basic physical parameter known to us, its unit Kelvin (K) is seven international basic units
One of, importance is seen some from this.No matter in our daily life, or in many important industrial production scenes
In, temperature is all a very crucial parameter, because temperature always has countless ties with some other states and result
Connection.For example, the temperature of bearing tends to the operating status for reflecting the component or even entire machine or system, thus can
With the temperature by monitoring bearing come whether judging that it works well.In more and more occasions, traditional temperature sensor
Part is no longer satisfied requirement, especially has the inherence for being difficult to overcome using thermocouple and thermal resistance as the temperature sensor of representative
Defect, such as: they will receive the disturbance of electric and magnetic fields to provide accurate temperature value；These are traditional simultaneously
Thermometer, which has to be come into full contact with object to be measured, can just provide temperature value, so that the temperature field to object to be measured carries out
Disturbance.Sensor based on optical medium can be solved these problems ideally.
In optics temp measuring method, the measurement that the fluorescence intensity ratio based on rare earth ion carries out temperature is before one kind has very much
The technology on way and potentiality.Rare earth ion has level structure abundant, and wherein energy level difference is in 200-2000cm-1Two energy levels claimed
Make thermal coupling energy level pair, the hot Statistical Distribution of Boltzmann is obeyed in the population distribution of this pair of of thermal coupling energy level pair, thus
Determining letter can be used between this ratio and temperature of a pair of of thermal coupling energy level to fluorescence caused by downward energy level transition
Number relationship description.Carrying out thermometric using the fluorescence intensity ratio technology of rare earth ion has a very strong anti-interference ability, but their institutes
It is commonly used in corresponding fluorescence spectral bands and our daily lifes and industrial production, the emission spectra of common white LED light source has very
It is seriously overlapped, thus unavoidably will receive the interference of these source of stray light, so as to cause the deviation of temperature measurement.
Summary of the invention
The purpose of the present invention is to solve existing rare earth ion fluorescence intensity ratio thermometrys will receive daily life
With commonly used in industrial production, the interference of common white LED light source the problem of, provide and resisted using converting purple light on thulium ion
The temp measuring method of white LED light source interference.
The present invention is according to the following steps using converting purple light on thulium ion to carry out the temp measuring method of anti-white LED light source interference
It carries out: one, preparing Yb3+And Tm3+The nanocrystal NaYF of ion doping4, obtain sample；Two, made using 980nm laser diode
Sample is excited for pump light source, changes the temperature of sample to obtain Tm under different temperatures3+Ion ultraviolet band it is upper
Conversion fluorescence, monitoring center's wavelength are located at two fluorescent belts of 290nm and 345nm, integrate to the intensity of two fluorescent belts,
And make the functional relation FIR=3.6*10 between the intensity rate and temperature of two fluorescent belts-4*exp(T/92.9)+1.55*
10-2；Three, sample is placed in environment to be measured, obtains the intensity rate of above-mentioned corresponding two fluorescent belts, is substituted into above-mentioned letter
It can be obtained ambient temperature value to be measured in number.
Laser diode of the present invention using emission center wavelength in 980nm is irradiated sample as excitation light source,
Wherein in 25mW or so, can ignore influences brought by the fuel factor of laser in this way the power control of laser diode.This hair
The bright Yb by after drying3+And Tm3+The nanocrystal NaYF of ion doping4Flaky material is pressed into facilitate the survey of subsequent alternating temperature spectrum
Amount.Wherein sheet sample with a thickness of 2mm, diameter 15mm, weight 0.6g, suppressing pressure used when sample is 8MPa,
Then sample is heated using temperature heating mantle and temperature controller, temperature range is 35 DEG C to 175 DEG C, temperature interval 10
℃.Wherein, 5min is stopped at each temperature spot so that print is by thermal balance, then utilizes the lens that focal length is 3.8cm will be glimmering
Light is focused, and the slit for projecting monochromator is received at light, and slit width therein is 1.5mm.Then pass through photomultiplier tube
It carries out the amplification of signal and is collected data in host computer by data collecting card.By the fluorescence intensity of 282-296nm wave band
It carries out integrating the intensity as 290nm fluorescence, the fluorescence intensity of 342-350nm wave band is subjected to integral as 345nm fluorescence
Intensity, then the fluorescence ratio of available the former and the latter, are denoted as FIR.Every 10 in 35 DEG C to 175 DEG C of temperature range
It DEG C can be obtained by a FIR numerical value, 15 FIR numerical value can be obtained in total.Using Origin data processing software by this 15
A FIR numerical value is fitted, and is found optimal approximation function, it is found that this 15 FIR numerical value can be carried out with functional relation below
It is fitted well:
FIR=A*exp (T/B)+C
Wherein A, B and C are constant, and T is kelvin rating.Final fitting result are as follows:
FIR=3.6*10-4*exp(T/92.9)+1.55*10-2。
The present invention is by selecting suitable host material NaYF4, and carry out sensitizer Yb3+The reasonable doping of ion, is sending out
Under the excitation for hitting the laser diode of a length of 980nm of cardiac wave, Tm is obtained3+The stronger upper conversion positioned at ultraviolet band of ion
Fluorescence, wherein the central wavelength of two involved fluorescent belts is respectively 290nm and 345nm.The intensity of the two fluorescent belts
Extraordinary functional relation is presented in 35 DEG C to 175 DEG C temperature ranges and temperature in ratio, from Tm3+290nm that ion is emitted and
It can be seen that all data point and FIR=3.6*10 in the intensity rate variation with temperature rule figure of 345nm fluorescent belt-4*
exp(T/92.9)+1.55*10-2It is fitted very good, related coefficient is greater than 0.998, shows that 290nm and 345nm fluorescent belt can be with
For carrying out the characterization of temperature.It thus can be used to carry out the measurement of temperature.Because the two fluorescent belts of 290nm and 345nm and
It is commonly used in daily life and industrial production, the emission spectrum of common white LED light source is not overlapped, it is thus possible to be resisted
The temperature measurement of white LED light source interference, to obtain more accurate result.
Detailed description of the invention
Fig. 1 is Yb of the invention3+And Tm3+The nanocrystal NaYF of ion doping4X ray diffracting spectrum；Wherein a is this
Invent the Yb of preparation3+And Tm3+The nanocrystal NaYF of ion doping4X ray diffracting spectrum, b be canonical reference curve；
Fig. 2 is the Yb involved in the present invention arrived3+And Tm3+The nanocrystal NaYF of ion doping4Room temperature fluorescence spectrum；Wherein
1 is Tm3+The up-conversion fluorescence band of the 290nm of ion, 2 be Tm3+The up-conversion fluorescence band of the 345nm of ion；
Fig. 3 is the Tm involved in the present invention arrived3+The intensity rate for the 290nm and 345nm fluorescent belt that ion is emitted is with temperature
The changing rule of degree；
Fig. 4 is the Tm involved in the present invention arrived3+290nm the and 345nm fluorescent belt and daily life, industry that ion is emitted
The comparison of the emission spectrum of common in production, common white LED light source；Wherein c be sample prepared by the present invention fluorescence Spectra,
D is white light LEDs emission spectra.
Specific embodiment
Specific embodiment 1: present embodiment carries out anti-white LED light source interference using conversion purple light on thulium ion
Temp measuring method is to sequentially include the following steps: one, preparation Yb3+And Tm3+The nanocrystal NaYF of ion doping4, obtain sample；Two,
Sample is excited as pump light source using 980nm laser diode, changes the temperature of sample to obtain different temperatures
Lower Tm3+The up-conversion fluorescence of ion ultraviolet band, monitoring center's wavelength is located at two fluorescent belts of 290nm and 345nm, to two
The intensity of fluorescent belt is integrated, and makes the functional relation FIR=3.6* between the intensity rate and temperature of two fluorescent belts
10-4*exp(T/92.9)+1.55*10-2, T is kelvin rating；Three, sample is placed in environment to be measured, obtains above-mentioned correspondence
Two fluorescent belts intensity rate, substituted into above-mentioned function and can be obtained ambient temperature value to be measured.
Laser diode of the present embodiment using emission center wavelength in 980nm shines sample as excitation light source
It penetrates, wherein in 25mW or so, can ignore influences brought by the fuel factor of laser in this way the power control of laser diode.This
Embodiment is by the Yb after drying3+And Tm3+The nanocrystal NaYF of ion doping4Flaky material is pressed into facilitate subsequent alternating temperature
The measurement of spectrum.Wherein sheet sample with a thickness of 2mm, diameter 15mm, weight 0.6g, pressure used is when suppressing sample
Then 8MPa heats sample using temperature heating mantle and temperature controller, temperature range is 35 DEG C to 175 DEG C, temperature interval
It is 10 DEG C.Wherein, 5min is stopped at each temperature spot so that print is by thermal balance, is then the lens of 3.8cm using focal length
Fluorescence is focused, the slit for projecting monochromator is received at light, and slit width therein is 1.5mm.Then pass through photoelectricity times
Increase pipe to carry out the amplification of signal and collect data in host computer by data collecting card.By the fluorescence of 282-296nm wave band
Intensity carries out integrating the intensity as 290nm fluorescence, and it is glimmering as 345nm that the fluorescence intensity of 342-350nm wave band is carried out integral
The intensity of light, then the fluorescence ratio of available the former and the latter, are denoted as FIR.It is every in 35 DEG C to 175 DEG C of temperature range
It can be obtained by a FIR numerical value every 10 DEG C, 15 FIR numerical value can be obtained in total.It will using Origin data processing software
This 15 FIR numerical value are fitted, and are found optimal approximation function, it is found that this 15 FIR numerical value can use functional relation below
It is fitted well:
FIR=A*exp (T/B)+C
Wherein A, B and C are constant, and T is kelvin rating.Final fitting result are as follows:
FIR=3.6*10-4*exp(T/92.9)+1.55*10-2。
Present embodiment is by selecting suitable host material NaYF4, and carry out sensitizer Yb3+The reasonable doping of ion,
In the transmission under the excitation of the laser diode of a length of 980nm of cardiac wave, Tm is obtained3+Ion is stronger positioned at the upper of ultraviolet band
Conversion fluorescence, wherein the central wavelength of two involved fluorescent belts is respectively 290nm and 345nm.The two fluorescent belts
Extraordinary functional relation is presented in 35 DEG C to 175 DEG C temperature ranges and temperature in intensity rate, from Tm3+What ion was emitted
It can be seen that all data point and FIR=in the intensity rate variation with temperature rule figure of 290nm and 345nm fluorescent belt
3.6*10-4*exp(T/92.9)+1.55*10-2It is fitted very good, related coefficient is greater than 0.998, shows 290nm and 345nm
Fluorescent belt can be used to carry out the characterization of temperature.It thus can be used to carry out the measurement of temperature.Because 290nm and 345nm this two
The emission spectrum of common, common white LED light source is not overlapped in a fluorescent belt and daily life and industrial production, thus
It is able to carry out the temperature measurement of anti-white LED light source interference, to obtain more accurate result.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: Yb in step 13+And Tm3+From
The nanocrystal NaYF of son doping4Preparation method be solvent-thermal method.It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: Yb in step 13+With
Tm3+The nanocrystal NaYF of ion doping4Preparation method specifically includes the following steps:
(1) under conditions of continuing magnetic force stirs and whole process leads to nitrogen protection gas, by 0.75mmol YbCl3·6H2O、
0.25mmol YbCl3·6H2O and 0.003mmol TmCl3·6H2O is added in the round bottom there-necked flask of 50mL, and 6mL is added
There-necked flask is then sealed and is heated to 160 DEG C of heat preservation 1h by oleic acid and 10mL octadecylene solvent；
(2) by 6mmol NaOH and 4mmol NH4F is added in the glass sample bottle of the methanol solution equipped with 20mL,
Continuing magnetic force stirs 0.5h at a temperature of 50 DEG C, obtains mixed solution A；
(3) there-necked flask of step (1) is cooled to 50 DEG C, and mixed solution A is added in there-necked flask, at such a temperature
Keep the temperature 0.5h；
(4) there-necked flask of step (3) is warming up to 70 DEG C and is open and keep the temperature 10min；
(5) there-necked flask of step (4) is warming up to 110 DEG C and is open and keep the temperature 10min；
(6) there-necked flask of step (5) is warming up to 300 DEG C and sealing thermal insulation 1h；
(7) there-necked flask of step (6) is cooled to room temperature, 30mL dehydrated alcohol is added and centrifugation obtains nanocrystal
NaYF4Sample；
(8) by nanocrystal NaYF4Sample stands for 24 hours i.e. completion in 70 DEG C of thermostatic drying chamber.Other and specific implementation
Mode one or two is identical.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: Yb in step 13+
And Tm3+The molar concentration of ion doping is respectively 25% and 0.3%.It is other identical as one of specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: institute in step 1
The Yb of preparation3+And Tm3+The nanocrystal NaYF of ion doping4For nano powder material.Other and specific embodiment one to four
One of it is identical.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: institute in step 1
The Yb of preparation3+And Tm3+The nanocrystal NaYF of ion doping4For hexagonal phase crystal structure.It is other with specific embodiment one to
One of five is identical.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: in step 2
The temperature range for changing sample is 35 DEG C~175 DEG C, is divided into 10 DEG C between changing every time.It is other with specific embodiment one to six it
One is identical.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: two fluorescent belts
Intensity rate and temperature between functional relation calculation method are as follows: the fluorescence intensity of 282-296nm wave band is integrated
As the intensity of 290nm fluorescence, the fluorescence intensity of 342-350nm wave band is carried out to integrate the intensity as 345nm fluorescence, then
The fluorescence ratio of the former and the latter are obtained, FIR is denoted as；One is just obtained every 10 DEG C in 35 DEG C to 175 DEG C of temperature range
FIR numerical value obtains 15 FIR numerical value altogether；This 15 FIR numerical value are fitted using Origin data processing software, are obtained
Optimal approximation function FIR=A*exp (T/B)+C；Wherein A, B and C are constant, and T is kelvin rating；Final fitting knot
Fruit are as follows: FIR=3.6*10-4*exp(T/92.9)+1.55*10-2.It is other identical as one of specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: Tm in step 23+
The up-conversion fluorescence of the ultraviolet band of ion refers to that central wavelength is located at two fluorescent belts of 290nm and 345nm, derives from Tm3+
Ion1I6Energy level to3F4With3H6The transition of energy level.It is other identical as one of specific embodiment one to eight.
Beneficial effects of the present invention are verified by following embodiment:
Embodiment one: the temp measuring method that the present embodiment carries out anti-white LED light source interference using purple light is converted on thulium ion
It is to sequentially include the following steps: one, preparation Yb3+And Tm3+The nanocrystal NaYF of ion doping4, obtain sample；Two, 980nm is utilized
Laser diode excites sample as pump light source, changes the temperature of sample to obtain Tm under different temperatures3+Ion
The up-conversion fluorescence of ultraviolet band, monitoring center's wavelength are located at two fluorescent belts of 290nm and 345nm, to two fluorescent belts
Intensity is integrated, and makes the functional relation FIR=3.6*10 between the intensity rate and temperature of two fluorescent belts-4*exp
(T/92.9)+1.55*10-2, T is kelvin rating；Three, sample is placed in environment to be measured, acquisition above-mentioned corresponding two glimmering
The intensity rate of light belt is substituted into above-mentioned function and can be obtained ambient temperature value to be measured.
By the Yb after drying in the present embodiment3+And Tm3+The nanocrystal NaYF of ion doping4Flaky material is pressed into convenient
The measurement of subsequent alternating temperature spectrum.Wherein sheet sample with a thickness of 2mm, diameter 15mm, weight 0.6g, suppress sample when institute
Pressure is 8MPa.
Laser diode in the present embodiment using emission center wavelength in 980nm shines sample as excitation light source
It penetrates, wherein in 25mW or so, can ignore influences brought by the fuel factor of laser in this way the power control of laser diode.
Yb in step 13+And Tm3+The molar concentration of ion doping is respectively 25% and 0.3%.
Yb in step 13+And Tm3+The nanocrystal NaYF of ion doping4Preparation method specifically includes the following steps:
(1) under conditions of continuing magnetic force stirs and whole process leads to nitrogen protection gas, by 0.75mmol YbCl3·6H2O、
0.25mmol YbCl3·6H2O and 0.003mmol TmCl3·6H2O is added in the round bottom there-necked flask of 50mL, and 6mL is added
There-necked flask is then sealed and is heated to 160 DEG C of heat preservation 1h by oleic acid and 10mL octadecylene solvent；
(2) by 6mmol NaOH and 4mmol NH4F is added in the glass sample bottle of the methanol solution equipped with 20mL,
Continuing magnetic force stirs 0.5h at a temperature of 50 DEG C, obtains mixed solution A；
(3) there-necked flask of step (1) is cooled to 50 DEG C, and mixed solution A is added in there-necked flask, at such a temperature
Keep the temperature 0.5h；
(4) there-necked flask of step (3) is warming up to 70 DEG C and is open and keep the temperature 10min；
(5) there-necked flask of step (4) is warming up to 110 DEG C and is open and keep the temperature 10min；
(6) there-necked flask of step (5) is warming up to 300 DEG C and sealing thermal insulation 1h；
(7) there-necked flask of step (6) is cooled to room temperature, 30mL dehydrated alcohol is added and centrifugation obtains nanocrystal
NaYF4Sample；
(8) by nanocrystal NaYF4Sample stands for 24 hours i.e. completion in 70 DEG C of thermostatic drying chamber.
The temperature range of change sample in step 2 is 35 DEG C~175 DEG C, is divided into 10 DEG C between changing every time.
Fig. 1 is the Yb involved in the present invention arrived3+And Tm3+The nanocrystal NaYF of ion doping4X ray diffracting spectrum.
By comparing Yb3+And Tm3+The nanocrystal NaYF of ion doping4All diffractive features peaks and the NaYF from hexagonal phase4
The diffraction maximum of the standard card of material finds that the position of all diffraction maximums of prepared sample all meets very well, shows success
Ground is prepared for the Yb of hexagonal phase3+And Tm3+The nanocrystal NaYF of ion doping4, be conducive to Tm3+The up-conversion fluorescence of ion
Transmitting.
Fig. 2 show Yb3+And Tm3+The nanocrystal NaYF of ion doping4Room temperature fluorescence spectrum, it can be seen that in middle cardiac wave
There is fluorescent belt at two at a length of 290nm and 345nm, they are respectively from Tm3+Ion1I6Energy level to3F4With3H6The jump of energy level
It moves.It is able to observe that the signal-to-noise ratio of the two fluorescent belts is all relatively good, thus is conducive to actual temperature measurement.In the present embodiment
Sample is heated using temperature heating mantle and temperature controller, temperature range is 35 DEG C to 175 DEG C, and temperature interval is 10 DEG C.Its
In, 5min is stopped at each temperature spot so that print is by thermal balance.
In the present embodiment in sample after by thermal balance, then fluorescence is focused using the lens that focal length is 3.8cm,
The slit for projecting monochromator is received at light, and slit width therein is 1.5mm.Then putting for signal is carried out by photomultiplier tube
Greatly and data are collected in host computer by data collecting card.
The fluorescence intensity of 282-296nm wave band is carried out to integrate the intensity as 290nm fluorescence, by 342-350nm wave band
Fluorescence intensity carry out integrating intensity as 345nm fluorescence, then the fluorescence ratio of available the former and the latter, are denoted as
FIR.It can be obtained by a FIR numerical value every 10 DEG C in 35 DEG C to 175 DEG C of temperature range, 15 can be obtained in total
FIR numerical value.
This 15 FIR numerical value are fitted using Origin data processing software, optimal approximation function is found, finds this
15 FIR numerical value can be fitted well with functional relation below:
FIR=A*exp (T/B)+C
Wherein A, B and C are constant, and T is kelvin rating.Final fitting result are as follows:
FIR=3.6*10-4*exp(T/92.9)+1.55*10-2。
As the result is shown in Fig. 3.All data points and above-mentioned functional relation are fitted very as we can see from the figure
Good, related coefficient is greater than 0.998, shows that 290nm and 345nm fluorescent belt can be used to carry out the characterization of temperature.Obtaining this
After functional relation, so that it may use Yb3+And Tm3+The nanocrystal NaYF of ion doping4It is measured to carry out the temperature of foreign environment,
After the intensity rate for obtaining 290nm and 345nm fluorescent belt in another environment, it is updated in above-mentioned functional relation
It counter can release the temperature value of environment.
Tm is shown in Fig. 43+Common, common white light LEDs in the UV fluorescence spectra of ion and daily life, industrial production
The comparison of the emission spectra of light source.It can be seen that in daily life, industrial production common, common white LED light source emission spectra
Positioned at this wave band of 410-700nm, and from Tm3+Two fluorescent belts of 290nm and 345nm of ion and white LED light source
Emission spectra is absolutely not overlapped, thus utilizes Tm3+Two fluorescent belts of 290nm and 345nm of ion carry out thermometric can be to avoid white
The interference of light LED light source, to obtain more accurately measuring.
Claims (9)
1. carrying out the temp measuring method of anti-white LED light source interference using ultraviolet light is converted on thulium ion, it is characterised in that be by with
Lower step carries out: one, preparing Yb3+And Tm3+The nanocrystal NaYF of ion doping4, obtain sample；Two, 980nm laser two is utilized
Pole pipe excites sample as pump light source, changes the temperature of sample to obtain Tm under different temperatures3+Ion ultraviolet waves
The up-conversion fluorescence of section, monitoring center's wavelength is located at two fluorescent belts of 290nm and 345nm, to the intensity of two fluorescent belts into
Row integral, and make the functional relation FIR=3.6*10 between the intensity rate and temperature of two fluorescent belts-4*exp(T/92.9)
+1.55*10-2, T is kelvin rating；Three, sample is placed in environment to be measured, obtains the strong of corresponding above-mentioned two fluorescent belt
Ratio is spent, is substituted into above-mentioned function and can be obtained ambient temperature value to be measured.
2. the thermometric side according to claim 1 for carrying out anti-white LED light source interference using ultraviolet light is converted on thulium ion
Method, it is characterised in that Yb in step 13+And Tm3+The nanocrystal NaYF of ion doping4Preparation method be solvent-thermal method.
3. the thermometric side according to claim 1 for carrying out anti-white LED light source interference using ultraviolet light is converted on thulium ion
Method, it is characterised in that Yb in step 13+And Tm3+The nanocrystal NaYF of ion doping4Preparation method specifically include following step
It is rapid:
(1) under conditions of continuing magnetic force stirs and whole process leads to nitrogen protection gas, by 0.75mmol YbCl3·6H2O、
0.25mmol YbCl3·6H2O and 0.003mmol TmCl3·6H2O is added in the round bottom there-necked flask of 50mL, and 6mL is added
There-necked flask is then sealed and is heated to 160 DEG C of heat preservation 1h by oleic acid and 10mL octadecylene solvent；
(2) by 6mmol NaOH and 4mmol NH4F is added in the glass sample bottle of the methanol solution equipped with 20mL, at 50 DEG C
At a temperature of continuing magnetic force stir 0.5h, obtain mixed solution A；
(3) there-necked flask of step (1) is cooled to 50 DEG C, and mixed solution A is added in there-necked flask, kept the temperature at such a temperature
0.5h；
(4) there-necked flask of step (3) is warming up to 70 DEG C and is open and keep the temperature 10min；
(5) there-necked flask of step (4) is warming up to 110 DEG C and is open and keep the temperature 10min；
(6) there-necked flask of step (5) is warming up to 300 DEG C and sealing thermal insulation 1h；
(7) there-necked flask of step (6) is cooled to room temperature, 30mL dehydrated alcohol is added and centrifugation obtains nanocrystal NaYF4Sample
Product；
(8) by nanocrystal NaYF4Sample stands for 24 hours i.e. completion in 70 DEG C of thermostatic drying chamber.
4. the thermometric side according to claim 1 for carrying out anti-white LED light source interference using ultraviolet light is converted on thulium ion
Method, it is characterised in that Yb in step 13+And Tm3+The molar concentration of ion doping is respectively 25% and 0.3%.
5. the thermometric side according to claim 1 for carrying out anti-white LED light source interference using ultraviolet light is converted on thulium ion
Method, it is characterised in that prepared Yb in step 13+And Tm3+The nanocrystal NaYF of ion doping4For nano powder material.
6. the thermometric side according to claim 1 for carrying out anti-white LED light source interference using ultraviolet light is converted on thulium ion
Method, it is characterised in that prepared Yb in step 13+And Tm3+The nanocrystal NaYF of ion doping4For hexagonal phase crystal structure.
7. the thermometric side according to claim 1 for carrying out anti-white LED light source interference using ultraviolet light is converted on thulium ion
Method, it is characterised in that the temperature range of the change sample in step 2 is 35 DEG C~175 DEG C, is divided into 10 DEG C between changing every time.
8. the thermometric side according to claim 1 for carrying out anti-white LED light source interference using ultraviolet light is converted on thulium ion
Method, it is characterised in that the calculation method of the functional relation between the intensity rate and temperature of two fluorescent belts are as follows: by 282-296nm
The fluorescence intensity of wave band carries out integrating the intensity as 290nm fluorescence, and the fluorescence intensity of 342-350nm wave band is carried out integral work
For the intensity of 345nm fluorescence, the fluorescence ratio of the former and the latter are then obtained, FIR is denoted as；35 DEG C to 175 DEG C of humidity province
It is interior that a FIR numerical value is just obtained every 10 DEG C, 15 FIR numerical value are obtained altogether；Using Origin data processing software by this 15
A FIR numerical value is fitted, and obtains optimal approximation function FIR=A*exp (T/B)+C；Wherein A, B and C are constant, and T is exhausted
To temperature value；Final fitting result are as follows: FIR=3.6*10-4*exp(T/92.9)+1.55*10-2。
9. the thermometric side according to claim 1 for carrying out anti-white LED light source interference using ultraviolet light is converted on thulium ion
Method, it is characterised in that Tm in step 23+The up-conversion fluorescence of the ultraviolet band of ion refer to central wavelength be located at 290nm and
Two fluorescent belts of 345nm derive from Tm3+Ion1I6Energy level to3F4With3H6The transition of energy level.
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