CN108441219A - A kind of upconverting fluorescent material preparation method of size tunable - Google Patents
A kind of upconverting fluorescent material preparation method of size tunable Download PDFInfo
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- CN108441219A CN108441219A CN201810217767.8A CN201810217767A CN108441219A CN 108441219 A CN108441219 A CN 108441219A CN 201810217767 A CN201810217767 A CN 201810217767A CN 108441219 A CN108441219 A CN 108441219A
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- 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
- C09K11/7772—Halogenides
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a kind of upconverting fluorescent material preparation methods of size tunable, include the following steps：Step 1, rare earth-iron-boron or rare earth acetic acid compound are added in container, add oleic acid, then heats, obtain the rare earth oleic acid presoma of clear；Sodium hydroxide and ammonium fluoride are added in low boiling point organic solvent, the sodium fluoride presoma of clear is obtained；Step 2, octadecylene is added into the rare earth oleic acid presoma of step 1, then heats；Step 3; the rare earth oleic acid presoma of step 2 is cooled down; sodium fluoride presoma is added in rare earth oleic acid presoma; reactant is heated up under protection of argon gas later simultaneously insulation reaction, waits for that after reaction, reaction mother liquor being cooled down; it is then centrifuged for that product is made to be precipitated out from solution; it washs later, the product after precipitation is washed, is dissolved in preserving or drying in organic solvent preserving.
Description
Technical field
The invention belongs to field of nanometer material technology, the upconverting fluorescent material preparation method of especially a kind of size tunable.
Background technology
Currently, fluorescence immune chromatography test strip is employed in the detection of mankind's relevant disease antigen-antibody, fluorescence
Immunochromatography technique has high sensitivity compared with traditional colloidal gold technique, and the range of linearity is wide, and can carry out quantitative detection
The advantages that.But current fluorescence para-immunity chromatography detection technique mainly turns fluorescent technique under, that is, passes through burst of ultraviolel
Luminescent substance (fluorescein, lanthanide series compound nanoparticle, quantum dot nano-particle etc.), then detect the visible light launched into
Row quantifies or qualitative analysis.Due to problem of fluorescent material itself, under turn the spy that class fluorescent technique is drifted in the prevalence of light
Property, the utilization which greatly limits fluorescence immune chromatography technology in the fields IVD.
Up-conversion refers to the visible light that can effectively absorb the near infrared light of long wavelength and launch short wavelength, can be inhaled
Receive then a kind of advanced luminescent material that lower energy photon launches high-energy photon.Compared with traditional downconversion fluorescent material, on
Changing luminous material has many advantages, such as that high chemical stability, low bio-toxicity and background fluorescence, tissue penetration depths are deeper.
Everybody is there are mainly two types of the upconverting fluorescent materials used at present：(1) grain size 30nm or so, pattern are uniformly received
Rice grain；(2) hundreds of nanometers of grain size, the irregular nano particle of pattern.The first material is small because of grain size, fluorescence is weak, is applied to
Height is required to detecting instrument when immunochromatography field, and sensitivity is low.Second of material is because pattern is irregular, therefore is being immunized
Race plate is not clean when chromatography, and signal-to-noise ratio is low, influences accuracy and the sensitivity of detection.
Invention content
The present invention using the upper conversion nano particle of two-step method synthesis, then by control rare earth ratio, oleic acid octadecylene dosage,
Reaction temperature and time, can controlling synthesis, 30-900nm uniform particle diameters are controllable, the uniform nano particle of pattern.This grain size
Greatly, the particle that pattern is uniform, luminous efficiency is high is more suitable for immunochromatography detection architecture, improves the sensitive of immunochromatography detection
Degree, accuracy, stability.
To solve the above-mentioned problems, the present invention proposes a kind of upconverting fluorescent material preparation method of size tunable.
The technical solution adopted in the present invention is：
A kind of upconverting fluorescent material preparation method of size tunable, includes the following steps：
Step 1, rare earth-iron-boron or rare earth acetic acid compound are added in container, add oleic acid, then heats,
Obtain rare earth-oleic acid presoma of clear；Sodium hydroxide and ammonium fluoride are added in low boiling point organic solvent, obtained clear
Clear bright sodium fluoride presoma；
Step 2, octadecylene is added into the rare earth of step 1-oleic acid presoma, then heats；
Step 3, the rare earth oleic acid presoma of step 2 is cooled down, sodium fluoride presoma is added in rare earth oleic acid presoma,
Reactant is heated up under protection of argon gas later simultaneously insulation reaction, is waited for that after reaction, reaction mother liquor being cooled down, is then centrifuged for making
Product is precipitated out from solution, is washed later, the product after precipitation is washed, is dissolved in preserving or drying in organic solvent
It is dry to preserve.
Rare earth-oleic acid presoma is prepared using two-step method, in the first step due to only existing rare earth compound and oleic acid, more
Be conducive to be stablized, be uniform, the sufficient rare earth-oleic acid presoma of dissolving.The upper conversion nano nucleus being synthesized by two-step process
For traditional one-step method, average grain diameter bigger, grain size evenly, and greatly reduce synthesis nanometer between different batches
The difference between batch of grain.
Further, the rare earth-iron-boron in the step 1, including (100-X-Y-Z) % yttriums, X% ytterbiums, Y% erbiums, Z%
Lutetium, X values 10-40, Y value 0.2-5, Z value 0-80.Content by regulating and controlling lutetium can control grain size, and content is higher, grain size
It is bigger, and then obtain the nano material for meeting demand.
Further, the heating temperature in the step 1 is 140-170 degrees Celsius, and heating time is 2-30 minutes.Herein
In temperature range and time, it is ensured that rare earth and elaidin reaction are abundant, are more advantageous to and are stablized, is uniform, dissolving sufficient rare earth-
Oleic acid presoma.
Further, the heating temperature in the step 2 is 140-170 degrees Celsius, and heating time is 2-30 minutes.Herein
In temperature range and time, it is ensured that rare earth-oleic acid presoma and octadecylene reaction are abundant, are more advantageous to and are stablized, is uniform, is molten
Solve sufficient rare earth-oleic acid presoma.
Further, reactant is warming up to 290-320 degrees Celsius and keeps the temperature 30-250 minutes in the step 3.Pass through tune
Section reaction temperature, reaction time can adjust grain size, and then obtain the nano material for meeting demand.
Preferably, the molar ratio of the oleic acid and rare earth compound that are added in the step 1 is 10:1 to 30:1, sodium hydroxide
Molar ratio with rare earth compound is 2.5:1, the molar ratio of ammonium fluoride and rare earth compound is 4:1.By adjusting oleic acid dosage
Grain size can be adjusted, and then obtains the nano material for meeting demand.
Preferably, the molar ratio of the octadecylene and rare earth compound that are added in the step 2 is 50:1 to 100：1.Pass through
Grain size can be adjusted by adjusting octadecylene dosage, and then obtain the nano material for meeting demand.
Preferably, the rare earth oleic acid presoma in the step 3 is cooled to 50 degrees Celsius, then under agitation by fluorine
Change sodium presoma to be added in rare earth oleic acid presoma, mixing time is 30 minutes, and washing times are 3-5 times.By stirring and washing
It washs, reactant can adequately be precipitated, and then improve the quantum of output of product.
The present invention compared with the existing technology has the following advantages and effect：
1, the present invention using two-step method prepares rare earth oleic acid presoma, in the first step due to only exist rare earth compound with
Oleic acid is more advantageous to and is stablized, is uniform, dissolving sufficient rare earth oleic acid presoma.The upper conversion being synthesized by two-step process is received
For traditional one-step method, average grain diameter bigger, grain size evenly, and are greatly reduced and are synthesized between different batches meter Jing He
The difference between batch of nano particle.
2, the present invention is used using the upper conversion nano particle of two-step method synthesis, then by control rare earth ratio, oleic acid octadecylene
Amount, reaction temperature and time, it can control that synthesis 30-900nm uniform particle diameters are controllable, the uniform nano particle of pattern.This grain
The particle that diameter is big, pattern is uniform, luminous efficiency is high is more suitable for immunochromatography detection architecture, improves the spirit of immunochromatography detection
Sensitivity, accuracy, stability.
Description of the drawings
The attached drawing constituted part of this application is used to provide further understanding of the present invention, schematic reality of the invention
Example and its explanation are applied for explaining the present invention, is not constituted improper limitations of the present invention.
Fig. 1 is the electron microscope under the 250nm of the present invention；
Fig. 2 is the electron microscope under the 500nm of the present invention；
Fig. 3 is the electron microscope under the 700nm of the present invention.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not
For limiting the present invention.
The technical solution adopted in the present invention is：
A kind of upconverting fluorescent material preparation method of size tunable, includes the following steps：
Step 1, rare earth-iron-boron or rare earth acetic acid compound are added in container, add oleic acid, then heats,
Obtain rare earth-oleic acid presoma of clear；Sodium hydroxide and ammonium fluoride are added in low boiling point organic solvent, obtained clear
Clear bright sodium fluoride presoma；
Step 2, octadecylene is added into the rare earth of step 1-oleic acid presoma, then heats；
Step 3, the rare earth oleic acid presoma of step 2 is cooled down, sodium fluoride presoma is added in rare earth oleic acid presoma,
Reactant is heated up under protection of argon gas later simultaneously insulation reaction, is waited for that after reaction, reaction mother liquor being cooled down, is then centrifuged for making
Product is precipitated out from solution, is washed later, the product after precipitation is washed, is dissolved in preserving or drying in organic solvent
It is dry to preserve.
Heretofore described rare earth-iron-boron or rare earth acetic acid compound, oleic acid, sodium hydroxide, ammonium fluoride low boiling point have
The source of solvent and organic solvent does not limit, using well known to those skilled in the art commercially available or homemade, rare earth
Chloride or rare earth acetic acid compound are made of following element：Yttrium (Y), ytterbium (Yb), erbium (Er), lutetium (Lu), are preferably in a proportion of
(100-X-Y-Z) % yttriums, X% ytterbiums, Y% erbiums, Z% lutetiums, X values 10-40, Y value 0.2-5, Z value 0-80；Adding in step 1
Hot temperature is preferably 140-170 degrees Celsius, and the time is 2-30 minutes；Heating temperature in step 2 is preferably 140-170 Celsius
Degree, time are 2-30 minutes；Reactant warming temperature is preferably 290-320 degrees Celsius and keeps the temperature 30-250 minutes in step 3；Step
The molar ratio of the oleic acid and rare earth compound that are added in rapid 1 is preferably 10:1 to 30:1, sodium hydroxide and rare earth compound rub
You are than preferably 2.5:1, the molar ratio of ammonium fluoride and rare earth compound is preferably 4:1；The octadecylene and rare earth being added in step 2
The molar ratio of compound is preferably 50:1 to 100：1.
It is described further with reference to embodiment.
Embodiment 1：
As shown in Figures 1 to 3, the upconverting fluorescent material preparation method of a kind of size tunable, which is characterized in that including following
Step：
Step 1, by a certain proportion of rare earth-iron-boron of 2mmol, rare earth-iron-boron includes 20% ytterbium (Yb), 2% erbium
(Er) and 78% lutetium (Lu) it, is added in three neck round bottom flask, adds 8ml oleic acid (OA), heat under the conditions of magnetic agitation
It to 140 degrees Celsius and is kept for 2 minutes, finally obtains rare earth-oleic acid presoma of clear；By the sodium hydroxide of 5mmol
(NaOH) it is added in 10ml methanol with the ammonium fluoride of 8mmol (NH4F), ultrasound is to obtaining the sodium fluoride presoma of clear；
Step 2,20ml octadecylenes (ODE) are added into the rare earth of step 1-oleic acid presoma, in magnetic agitation condition
Under be heated to 140 degrees Celsius and keep 2 minutes；
Step 3, after prepared by rare earth oleic acid (Ln-OA) presoma of step 2,50 degrees Celsius are first cooled to, then in magnetic
Under power stirring condition, sodium fluoride (NaF) presoma is slowly added to translate in rare earth oleic acid (Ln-OA) presoma, continuously
After stirring 30 minutes, reactant is warming up to 290 degrees Celsius of simultaneously insulation reaction 30 minutes under high-purity argon gas protection.Wait for reaction knot
Shu Hou, ethyl alcohol is added after reaction mother liquor is cooled down makes product Precipitation from solution, then centrifuges, repeatedly using absolute ethyl alcohol
Product is obtained after washing 3 times, and product is dissolved in hexamethylene.
The average grain diameter of obtained nano particle, size grade scale, batch between standard deviation it is as shown in table 1.
Table 1：
Embodiment 2：
The present embodiment is substantially the same manner as Example 1, and distinctive points are：In embodiment 2, the rare earth-iron-boron packet in step 1
Containing 20% ytterbium (Yb), 2% erbium (Er) and 78% yttrium (Y), the mass ratio of oleic acid and rare earth-iron-boron is 10:1；Ten in step 2
The mass ratio of eight alkene and rare earth-oleic acid presoma is 100:1；Reactant is warming up to 300 under high-purity argon gas protection in step 3
Degree Celsius and insulation reaction 60 minutes.
The average grain diameter of obtained nano particle is 32.7nm, and size grade scale difference is 1.8 in batch, and size grade scale difference is between batch
2.2。
Embodiment 3：
The present embodiment is substantially the same manner as Example 1, and distinctive points are：In embodiment 3, the quality of oleic acid and rare earth-iron-boron
Than being 30:1；The mass ratio of octadecylene and rare earth-oleic acid presoma in step 2 is 50:1；By reactant high-purity in step 3
320 degrees Celsius of simultaneously insulation reaction 240 minutes are warming up under argon gas protection.
The average grain diameter of obtained nano particle is 883.5nm, and size grade scale difference is 29.6 in batch, and size grade scale is poor between batch
It is 65.7.
Embodiment 4：
The present embodiment is substantially the same manner as Example 1, and distinctive points are：In embodiment 4, the rare earth-iron-boron packet in step 1
Containing 28% yttrium (Y), the mass ratio of 20% ytterbium (Yb), 2% erbium (Er), 50% lutetium (Lu), oleic acid and rare earth-iron-boron is 20:1；Step
The mass ratio of octadecylene and rare earth-oleic acid presoma in rapid 2 is 60:1；In step 3 by reactant under high-purity argon gas protection
It is warming up to 300 degrees Celsius of simultaneously insulation reaction 120 minutes.
The average grain diameter of obtained nano particle is 150.6nm, and size grade scale difference is 4.6 in batch, and size grade scale is poor between batch
It is 5.7.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of upconverting fluorescent material preparation method of size tunable, which is characterized in that include the following steps：
Step 1, rare earth-iron-boron or rare earth acetic acid compound are added in container, add oleic acid, then heat, obtains
The rare earth of clear-oleic acid presoma；Sodium hydroxide and ammonium fluoride are added in low boiling point organic solvent, it is saturating to obtain clarification
Bright sodium fluoride presoma；
Step 2, octadecylene is added into the rare earth of step 1-oleic acid presoma, then heats；
Step 3, the rare earth oleic acid presoma of step 2 is cooled down, sodium fluoride presoma is added in rare earth oleic acid presoma, later
Reactant is heated up under protection of argon gas simultaneously insulation reaction, is waited for that after reaction, reaction mother liquor being cooled down, is then centrifuged for making product
It is precipitated out from solution, washs later, the product after precipitation is washed is dissolved in preserving or drying in organic solvent protecting
It deposits.
2. the upconverting fluorescent material preparation method of size tunable according to claim 1, which is characterized in that the step
Rare earth-iron-boron in 1, including (100-X-Y-Z) % yttriums, X% ytterbiums, Y% erbiums, Z% lutetiums, X values 10-40, Y value 0.2-5, Z
Value 0-80.
3. the upconverting fluorescent material preparation method of size tunable according to claim 2, which is characterized in that the step
Heating temperature in 1 is 140-170 degrees Celsius, and heating time is 2-30 minutes.
4. upconverting fluorescent material preparation method according to claim 3, which is characterized in that the heating in the step 2
Temperature is 140-170 degrees Celsius, and heating time is 2-30 minutes.
5. the upconverting fluorescent material preparation method of size tunable according to claim 4, which is characterized in that the step
Reactant is warming up to 290-320 degrees Celsius and keeps the temperature 30-250 minutes in 3.
6. the upconverting fluorescent material preparation method of size tunable according to claim 5, which is characterized in that the step
The molar ratio of the oleic acid and rare earth compound that are added in 1 is 10:1 to 30:1, the molar ratio of sodium hydroxide and rare earth compound is
2.5:1, the molar ratio of ammonium fluoride and rare earth compound is 4:1.
7. the upconverting fluorescent material preparation method of size tunable according to claim 5, which is characterized in that the step
The molar ratio of the octadecylene and rare earth compound that are added in 2 is 50:1 to 100：1.
8. the upconverting fluorescent material preparation method of any size tunable of according to claim 6 or 7, which is characterized in that
Rare earth oleic acid presoma in the step 3 is cooled to 50 degrees Celsius, and then sodium fluoride presoma is added under agitation
In rare earth oleic acid presoma, mixing time is 30 minutes, and washing times are 3-5 times.
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| CN111171820A (en) * | 2019-12-23 | 2020-05-19 | 华南师范大学 | Etching method of rare earth fluoride up-conversion nanocrystal |
| CN112724977A (en) * | 2021-01-19 | 2021-04-30 | 吉林大学 | Size-adjustable beta-Na (LuY) F4Preparation method of intersoluble body nanocrystal |
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| CN112724977A (en) * | 2021-01-19 | 2021-04-30 | 吉林大学 | Size-adjustable beta-Na (LuY) F4Preparation method of intersoluble body nanocrystal |
| CN112724977B (en) * | 2021-01-19 | 2022-05-27 | 吉林大学 | Size-adjustable beta-Na (LuY) F4Preparation method of intersoluble body nanocrystal |
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