METHOD FOR PREPARING INDIUM PHOSPHIDE NANOCRYSTAL BY USING NOVEL PHOSPHORUS PRECURSOR AND INDIUM PHOSPHIDE NANOCRYSTAL PREPARED BY THE SAME | Matter42 Literature
Patent
Atlas literature
Patent
US 11,827,827 B2
METHOD FOR PREPARING INDIUM PHOSPHIDE NANOCRYSTAL BY USING NOVEL PHOSPHORUS PRECURSOR AND INDIUM PHOSPHIDE NANOCRYSTAL PREPARED BY THE SAME
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
FIG. 1 is a structure diagram showing a nanocrystal in a schematic example of the present application;
FIG. 2
FIG. 2 shows a transmission electron microscopy (TEM) of a nanocrystal in example 15;
FIG. 3
FIG. 3 shows a fluorescence emission spectrum of the nanocrystal in example 15.
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
4 independent · 15 dependent
1
IndependentInPM-(O-C≡P)nZn precursor
A preparation method of an indium phosphide nanoc-rystal, comprising a step of: using M-(O—C≡P)n as one of reaction precursors, wherein, M is element Na, Li, K, Zn or Ga, and n is a valence state of the M element; subjecting a solution comprising an In precursor, M-(O—C≡P)n, an optional Zn precursor and a solvent to high temperature treatment, thus obtaining an InP nanocrystal core.
2
Dependent← claim 1M-(O-C≡P)nZn precursor
The preparation method according to claim 1, wherein the reaction precursors further comprise an In precursor; and/or, the reaction precursors further comprise a Zn precursor.
3
Dependent← claim 1InP
The preparation method according to claim 1, wherein the InP nanocrystal comprises elements M, In and P, and an optional Zn element.
4
Dependent← claim 1InP
The preparation method according to claim 1, wherein, the high temperature treatment has a temperature within 150-340° C.
5
Dependent← claim 1InP
The preparation method according to claim 1, com-prising a step of: coating a shell on the nanocrystal core; and/or, wherein the solvent is a coordination compound; the coordination compound is amine or carboxylic acid.
6
Dependent← claim 1InP
The preparation method according to claim 1, wherein the high temperature treatment has a temperature within 150-300° C.
7
IndependentInPM-(O-C≡P)nZn precursorInP
A preparation method of a near-infrared InP nanocrys-tal, comprising the following steps: S1, obtaining a first solution system comprising an In precursor and an optional Zn precursor, and a second solution system comprising M-(O—C≡P)n, as a P precursor, wherein M is element Na, Li, K, Zn or Ga; S2, mixing the first solution system with the second solution system for reaction at a predetermined tem-perature to obtain the near-infrared InP nanocrystal; wherein the predetermined temperature has a range of 180-320° C., the first solution system comprises the In precursor, the optional Zn precursor and a first organic solvent dispersing the In precursor; and the second solution system comprises the P precursor and a second organic solvent dispersing the P precursor; the first organic solvent is different from the second organic solvent; and the second organic solvent has a boiling point lower than the predetermined temperature.
8
Dependent← claim 7
The preparation method according to claim 7, wherein the second organic solvent has a boiling point at least 30° C. lower than the predetermined temperature.
9
Dependent← claim 7
The preparation method according to claim 7, wherein the second organic solvent has a boiling point lower than or equal to 150° C.
The preparation method according to claim 7, wherein the In precursor is an indium halide; the first organic solvent is at least one of saturated or unsaturated amines having a carbon number not lower than 6, or carboxylic acids; and/or, the first solution system further comprises the Zn precursor; and/or, the shell of the nanocrystal comprises at least one of ZnS, ZnSe, and ZnSeS.
11
Dependent← claim 7InP
The preparation method according to claim 7, wherein the synthetic method further comprises a step S3, adding a precursor substance demanded for the synthesis of a shell of the nanocrystal to the reaction system of the S₂ step, and forming a shell on a surface of the near-infrared InP nanoc-rystal, so that the near-infrared InP nanocrystal has a fluo-rescence emission peak within 700-900 nm.
12
Dependent← claim 7
The preparation method according to claim 7, wherein the second organic solvent has a boiling point of 60-150° C.; and/or, the second organic solvent comprises at least one of benzene, methylbenzene, cyclohexane, n-hexane, n-heptane, normal octane, tetrahydrofuran and chloroform.
13
IndependentInPM-(O-C≡P)nInP
A preparation method of an red-emitting InP nanoc-rystal, comprising steps of: S1, mixing the In precursor and P precursor M-(O— C≡P)n, with an organic solvent for reaction at a first temperature, and thermally insulating for a period of time to obtain an InP nanocrystal core solution, wherein M is element Na, Li, K, Zn or Ga; S2, rapidly heating the InP nanocrystal core solution up to a second tem-perature and thermally insulating for a period of time; S3, adding a precusor substance demanded for the synthesis of a shell of the nanocrystal to the reaction system of the S₂ step to obtain the red-emitting InP nanocrystal, wherein the red-emitting InP nanocrystal has a fluorescence emission peak within 580-670 nm.
14
Dependent← claim 13
The preparation method according to claim 13, wherein the first temperature ranges from 110-160° C;and/or, the second temperature ranges from 280-340° C.
15
Dependent← claim 13
The preparation method according to claim 13, wherein in the S2, the InP nanocrystal core solution is rapidly heated up to the second temperature, keeping for at least 10 min.
16
Dependent← claim 13Zn precursorZnSZnSeZnSeS
The preparation method according to claim 13, wherein the organic solvent is selected from at least one of saturated or unsaturated amines having a carbon number not lower than 6, or carboxylic acids; and/or, the InP nanocrystal core solution optionally comprises a first Zn precursor, and the first Zn precursor is selected from a Zn halide; and/or, the shell of the nanocrystal comprises at least one of ZnS, ZnSe, and ZnSeS.
17
IndependentInPM-(O-C≡P)nInP
A preparation method of a cyan-emitting InP nanoc-rystal, comprising the following steps: S1, mixing the In precursor and P precursor M-(O— C≡P)n, with an organic solvent for reaction at a first temperature to obtain an InP nanocrystal core solution, wherein M is element Na, Li, K, Zn or Ga; S2, adding a cationic precursor to the InP nanocrystal core solution to form a first mixed solution at the first temperature; S3, adding a anionic precursor to the first mixed solution; wherein, the cationic precursor is reacted with the anionic precursor to coat a shell on the InP nanoc-rystal core, thus obtaining the cyan-emitting InP nanoc-rystal; the cyan-emitting InP nanocrystal has a fluores-cence emission peak within 460-500 nm; and wherein, B₂ the second temperature is greater than the first tem-perature.
18
Dependent← claim 17
The preparation method according to claim 17, wherein the first temperature ranges from 110-160° C;and/or, the second temperature ranges from 160-240° C.
19
Dependent← claim 17Zn precursor
The preparation method according to claim 17, wherein the organic solvent is selected from at least one of saturated or unsaturated amines having a carbon number not lower than 6, or carboxylic acids; and/or, the InP nanocrystal core solution optionally comprises a first Zn precursor, and the first Zn precursor is selected from a Zn halide; and/or, a ratio of the Zn cationic precursor in the step S₂ to the In precursor in the step S₁ is (8-40):1 according to a molar ratio; and/or, the cationic precursor is a second Zn precursor, and the second Zn precursor is selected from zinc carboxylate, or an organic zinc reagent; and/or, the anionic precursor is at least one of an S precursor and Se precursor. ∗ ∗ ∗ ∗ ∗
Materials
Materials described outside the worked examples.
InP nanocrystal
InP
Synthesis Product
M-(O—C≡P)n phosphorus precursor
M-(O-C≡P)n
Phosphorus Precursor
Zn precursor
Process steps
Additional fabrication and treatment steps described in the patent.
1
Colloidal Nanocrystal Synthesis
Step 1
Temperature
150, 340°C
Process details
method:high temperature treatment
solvent:
Characterization
Measurements and analyses referenced in the patent, with their drawing references.
tem
TEM
FIG. 2 shows a transmission electron microscopy (TEM) of a nanocrystal in example 15;
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
FIG. 1 is a structure diagram showing a nanocrystal in a schematic example of the present application;
FIG. 2
FIG. 2 shows a transmission electron microscopy (TEM) of a nanocrystal in example 15;
FIG. 3
FIG. 3 shows a fluorescence emission spectrum of the nanocrystal in example 15.
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
4 independent · 15 dependent
1
IndependentInPM-(O-C≡P)nZn precursor
A preparation method of an indium phosphide nanoc-rystal, comprising a step of: using M-(O—C≡P)n as one of reaction precursors, wherein, M is element Na, Li, K, Zn or Ga, and n is a valence state of the M element; subjecting a solution comprising an In precursor, M-(O—C≡P)n, an optional Zn precursor and a solvent to high temperature treatment, thus obtaining an InP nanocrystal core.
2
Dependent← claim 1M-(O-C≡P)nZn precursor
The preparation method according to claim 1, wherein the reaction precursors further comprise an In precursor; and/or, the reaction precursors further comprise a Zn precursor.
3
Dependent← claim 1InP
The preparation method according to claim 1, wherein the InP nanocrystal comprises elements M, In and P, and an optional Zn element.
4
Dependent← claim 1InP
The preparation method according to claim 1, wherein, the high temperature treatment has a temperature within 150-340° C.
5
Dependent← claim 1InP
The preparation method according to claim 1, com-prising a step of: coating a shell on the nanocrystal core; and/or, wherein the solvent is a coordination compound; the coordination compound is amine or carboxylic acid.
6
Dependent← claim 1InP
The preparation method according to claim 1, wherein the high temperature treatment has a temperature within 150-300° C.
7
IndependentInPM-(O-C≡P)nZn precursorInP
A preparation method of a near-infrared InP nanocrys-tal, comprising the following steps: S1, obtaining a first solution system comprising an In precursor and an optional Zn precursor, and a second solution system comprising M-(O—C≡P)n, as a P precursor, wherein M is element Na, Li, K, Zn or Ga; S2, mixing the first solution system with the second solution system for reaction at a predetermined tem-perature to obtain the near-infrared InP nanocrystal; wherein the predetermined temperature has a range of 180-320° C., the first solution system comprises the In precursor, the optional Zn precursor and a first organic solvent dispersing the In precursor; and the second solution system comprises the P precursor and a second organic solvent dispersing the P precursor; the first organic solvent is different from the second organic solvent; and the second organic solvent has a boiling point lower than the predetermined temperature.
8
Dependent← claim 7
The preparation method according to claim 7, wherein the second organic solvent has a boiling point at least 30° C. lower than the predetermined temperature.
9
Dependent← claim 7
The preparation method according to claim 7, wherein the second organic solvent has a boiling point lower than or equal to 150° C.
The preparation method according to claim 7, wherein the In precursor is an indium halide; the first organic solvent is at least one of saturated or unsaturated amines having a carbon number not lower than 6, or carboxylic acids; and/or, the first solution system further comprises the Zn precursor; and/or, the shell of the nanocrystal comprises at least one of ZnS, ZnSe, and ZnSeS.
11
Dependent← claim 7InP
The preparation method according to claim 7, wherein the synthetic method further comprises a step S3, adding a precursor substance demanded for the synthesis of a shell of the nanocrystal to the reaction system of the S₂ step, and forming a shell on a surface of the near-infrared InP nanoc-rystal, so that the near-infrared InP nanocrystal has a fluo-rescence emission peak within 700-900 nm.
12
Dependent← claim 7
The preparation method according to claim 7, wherein the second organic solvent has a boiling point of 60-150° C.; and/or, the second organic solvent comprises at least one of benzene, methylbenzene, cyclohexane, n-hexane, n-heptane, normal octane, tetrahydrofuran and chloroform.
13
IndependentInPM-(O-C≡P)nInP
A preparation method of an red-emitting InP nanoc-rystal, comprising steps of: S1, mixing the In precursor and P precursor M-(O— C≡P)n, with an organic solvent for reaction at a first temperature, and thermally insulating for a period of time to obtain an InP nanocrystal core solution, wherein M is element Na, Li, K, Zn or Ga; S2, rapidly heating the InP nanocrystal core solution up to a second tem-perature and thermally insulating for a period of time; S3, adding a precusor substance demanded for the synthesis of a shell of the nanocrystal to the reaction system of the S₂ step to obtain the red-emitting InP nanocrystal, wherein the red-emitting InP nanocrystal has a fluorescence emission peak within 580-670 nm.
14
Dependent← claim 13
The preparation method according to claim 13, wherein the first temperature ranges from 110-160° C;and/or, the second temperature ranges from 280-340° C.
15
Dependent← claim 13
The preparation method according to claim 13, wherein in the S2, the InP nanocrystal core solution is rapidly heated up to the second temperature, keeping for at least 10 min.
16
Dependent← claim 13Zn precursorZnSZnSeZnSeS
The preparation method according to claim 13, wherein the organic solvent is selected from at least one of saturated or unsaturated amines having a carbon number not lower than 6, or carboxylic acids; and/or, the InP nanocrystal core solution optionally comprises a first Zn precursor, and the first Zn precursor is selected from a Zn halide; and/or, the shell of the nanocrystal comprises at least one of ZnS, ZnSe, and ZnSeS.
17
IndependentInPM-(O-C≡P)nInP
A preparation method of a cyan-emitting InP nanoc-rystal, comprising the following steps: S1, mixing the In precursor and P precursor M-(O— C≡P)n, with an organic solvent for reaction at a first temperature to obtain an InP nanocrystal core solution, wherein M is element Na, Li, K, Zn or Ga; S2, adding a cationic precursor to the InP nanocrystal core solution to form a first mixed solution at the first temperature; S3, adding a anionic precursor to the first mixed solution; wherein, the cationic precursor is reacted with the anionic precursor to coat a shell on the InP nanoc-rystal core, thus obtaining the cyan-emitting InP nanoc-rystal; the cyan-emitting InP nanocrystal has a fluores-cence emission peak within 460-500 nm; and wherein, B₂ the second temperature is greater than the first tem-perature.
18
Dependent← claim 17
The preparation method according to claim 17, wherein the first temperature ranges from 110-160° C;and/or, the second temperature ranges from 160-240° C.
19
Dependent← claim 17Zn precursor
The preparation method according to claim 17, wherein the organic solvent is selected from at least one of saturated or unsaturated amines having a carbon number not lower than 6, or carboxylic acids; and/or, the InP nanocrystal core solution optionally comprises a first Zn precursor, and the first Zn precursor is selected from a Zn halide; and/or, a ratio of the Zn cationic precursor in the step S₂ to the In precursor in the step S₁ is (8-40):1 according to a molar ratio; and/or, the cationic precursor is a second Zn precursor, and the second Zn precursor is selected from zinc carboxylate, or an organic zinc reagent; and/or, the anionic precursor is at least one of an S precursor and Se precursor. ∗ ∗ ∗ ∗ ∗
Materials
Materials described outside the worked examples.
InP nanocrystal
InP
Synthesis Product
M-(O—C≡P)n phosphorus precursor
M-(O-C≡P)n
Phosphorus Precursor
Zn precursor
Process steps
Additional fabrication and treatment steps described in the patent.
1
Colloidal Nanocrystal Synthesis
Step 1
Temperature
150, 340°C
Process details
method:high temperature treatment
solvent:
Characterization
Measurements and analyses referenced in the patent, with their drawing references.
tem
TEM
FIG. 2 shows a transmission electron microscopy (TEM) of a nanocrystal in example 15;
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
FIG. 1 is a structure diagram showing a nanocrystal in a schematic example of the present application;
FIG. 2
FIG. 2 shows a transmission electron microscopy (TEM) of a nanocrystal in example 15;
FIG. 3
FIG. 3 shows a fluorescence emission spectrum of the nanocrystal in example 15.
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
4 independent · 15 dependent
1
IndependentInPM-(O-C≡P)nZn precursor
A preparation method of an indium phosphide nanoc-rystal, comprising a step of: using M-(O—C≡P)n as one of reaction precursors, wherein, M is element Na, Li, K, Zn or Ga, and n is a valence state of the M element; subjecting a solution comprising an In precursor, M-(O—C≡P)n, an optional Zn precursor and a solvent to high temperature treatment, thus obtaining an InP nanocrystal core.
2
Dependent← claim 1M-(O-C≡P)nZn precursor
The preparation method according to claim 1, wherein the reaction precursors further comprise an In precursor; and/or, the reaction precursors further comprise a Zn precursor.
3
Dependent← claim 1InP
The preparation method according to claim 1, wherein the InP nanocrystal comprises elements M, In and P, and an optional Zn element.
4
Dependent← claim 1InP
The preparation method according to claim 1, wherein, the high temperature treatment has a temperature within 150-340° C.
5
Dependent← claim 1InP
The preparation method according to claim 1, com-prising a step of: coating a shell on the nanocrystal core; and/or, wherein the solvent is a coordination compound; the coordination compound is amine or carboxylic acid.
6
Dependent← claim 1InP
The preparation method according to claim 1, wherein the high temperature treatment has a temperature within 150-300° C.
7
IndependentInPM-(O-C≡P)nZn precursorInP
A preparation method of a near-infrared InP nanocrys-tal, comprising the following steps: S1, obtaining a first solution system comprising an In precursor and an optional Zn precursor, and a second solution system comprising M-(O—C≡P)n, as a P precursor, wherein M is element Na, Li, K, Zn or Ga; S2, mixing the first solution system with the second solution system for reaction at a predetermined tem-perature to obtain the near-infrared InP nanocrystal; wherein the predetermined temperature has a range of 180-320° C., the first solution system comprises the In precursor, the optional Zn precursor and a first organic solvent dispersing the In precursor; and the second solution system comprises the P precursor and a second organic solvent dispersing the P precursor; the first organic solvent is different from the second organic solvent; and the second organic solvent has a boiling point lower than the predetermined temperature.
8
Dependent← claim 7
The preparation method according to claim 7, wherein the second organic solvent has a boiling point at least 30° C. lower than the predetermined temperature.
9
Dependent← claim 7
The preparation method according to claim 7, wherein the second organic solvent has a boiling point lower than or equal to 150° C.
The preparation method according to claim 7, wherein the In precursor is an indium halide; the first organic solvent is at least one of saturated or unsaturated amines having a carbon number not lower than 6, or carboxylic acids; and/or, the first solution system further comprises the Zn precursor; and/or, the shell of the nanocrystal comprises at least one of ZnS, ZnSe, and ZnSeS.
11
Dependent← claim 7InP
The preparation method according to claim 7, wherein the synthetic method further comprises a step S3, adding a precursor substance demanded for the synthesis of a shell of the nanocrystal to the reaction system of the S₂ step, and forming a shell on a surface of the near-infrared InP nanoc-rystal, so that the near-infrared InP nanocrystal has a fluo-rescence emission peak within 700-900 nm.
12
Dependent← claim 7
The preparation method according to claim 7, wherein the second organic solvent has a boiling point of 60-150° C.; and/or, the second organic solvent comprises at least one of benzene, methylbenzene, cyclohexane, n-hexane, n-heptane, normal octane, tetrahydrofuran and chloroform.
13
IndependentInPM-(O-C≡P)nInP
A preparation method of an red-emitting InP nanoc-rystal, comprising steps of: S1, mixing the In precursor and P precursor M-(O— C≡P)n, with an organic solvent for reaction at a first temperature, and thermally insulating for a period of time to obtain an InP nanocrystal core solution, wherein M is element Na, Li, K, Zn or Ga; S2, rapidly heating the InP nanocrystal core solution up to a second tem-perature and thermally insulating for a period of time; S3, adding a precusor substance demanded for the synthesis of a shell of the nanocrystal to the reaction system of the S₂ step to obtain the red-emitting InP nanocrystal, wherein the red-emitting InP nanocrystal has a fluorescence emission peak within 580-670 nm.
14
Dependent← claim 13
The preparation method according to claim 13, wherein the first temperature ranges from 110-160° C;and/or, the second temperature ranges from 280-340° C.
15
Dependent← claim 13
The preparation method according to claim 13, wherein in the S2, the InP nanocrystal core solution is rapidly heated up to the second temperature, keeping for at least 10 min.
16
Dependent← claim 13Zn precursorZnSZnSeZnSeS
The preparation method according to claim 13, wherein the organic solvent is selected from at least one of saturated or unsaturated amines having a carbon number not lower than 6, or carboxylic acids; and/or, the InP nanocrystal core solution optionally comprises a first Zn precursor, and the first Zn precursor is selected from a Zn halide; and/or, the shell of the nanocrystal comprises at least one of ZnS, ZnSe, and ZnSeS.
17
IndependentInPM-(O-C≡P)nInP
A preparation method of a cyan-emitting InP nanoc-rystal, comprising the following steps: S1, mixing the In precursor and P precursor M-(O— C≡P)n, with an organic solvent for reaction at a first temperature to obtain an InP nanocrystal core solution, wherein M is element Na, Li, K, Zn or Ga; S2, adding a cationic precursor to the InP nanocrystal core solution to form a first mixed solution at the first temperature; S3, adding a anionic precursor to the first mixed solution; wherein, the cationic precursor is reacted with the anionic precursor to coat a shell on the InP nanoc-rystal core, thus obtaining the cyan-emitting InP nanoc-rystal; the cyan-emitting InP nanocrystal has a fluores-cence emission peak within 460-500 nm; and wherein, B₂ the second temperature is greater than the first tem-perature.
18
Dependent← claim 17
The preparation method according to claim 17, wherein the first temperature ranges from 110-160° C;and/or, the second temperature ranges from 160-240° C.
19
Dependent← claim 17Zn precursor
The preparation method according to claim 17, wherein the organic solvent is selected from at least one of saturated or unsaturated amines having a carbon number not lower than 6, or carboxylic acids; and/or, the InP nanocrystal core solution optionally comprises a first Zn precursor, and the first Zn precursor is selected from a Zn halide; and/or, a ratio of the Zn cationic precursor in the step S₂ to the In precursor in the step S₁ is (8-40):1 according to a molar ratio; and/or, the cationic precursor is a second Zn precursor, and the second Zn precursor is selected from zinc carboxylate, or an organic zinc reagent; and/or, the anionic precursor is at least one of an S precursor and Se precursor. ∗ ∗ ∗ ∗ ∗
Materials
Materials described outside the worked examples.
InP nanocrystal
InP
Synthesis Product
M-(O—C≡P)n phosphorus precursor
M-(O-C≡P)n
Phosphorus Precursor
Zn precursor
Process steps
Additional fabrication and treatment steps described in the patent.
1
Colloidal Nanocrystal Synthesis
Step 1
Temperature
150, 340°C
Process details
method:high temperature treatment
solvent:
Characterization
Measurements and analyses referenced in the patent, with their drawing references.
tem
TEM
FIG. 2 shows a transmission electron microscopy (TEM) of a nanocrystal in example 15;
Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1
FIG. 1 is a structure diagram showing a nanocrystal in a schematic example of the present application;
FIG. 2
FIG. 2 shows a transmission electron microscopy (TEM) of a nanocrystal in example 15;
FIG. 3
FIG. 3 shows a fluorescence emission spectrum of the nanocrystal in example 15.
Claims
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
4 independent · 15 dependent
1
IndependentInPM-(O-C≡P)nZn precursor
A preparation method of an indium phosphide nanoc-rystal, comprising a step of: using M-(O—C≡P)n as one of reaction precursors, wherein, M is element Na, Li, K, Zn or Ga, and n is a valence state of the M element; subjecting a solution comprising an In precursor, M-(O—C≡P)n, an optional Zn precursor and a solvent to high temperature treatment, thus obtaining an InP nanocrystal core.
2
Dependent← claim 1M-(O-C≡P)nZn precursor
The preparation method according to claim 1, wherein the reaction precursors further comprise an In precursor; and/or, the reaction precursors further comprise a Zn precursor.
3
Dependent← claim 1InP
The preparation method according to claim 1, wherein the InP nanocrystal comprises elements M, In and P, and an optional Zn element.
4
Dependent← claim 1InP
The preparation method according to claim 1, wherein, the high temperature treatment has a temperature within 150-340° C.
5
Dependent← claim 1InP
The preparation method according to claim 1, com-prising a step of: coating a shell on the nanocrystal core; and/or, wherein the solvent is a coordination compound; the coordination compound is amine or carboxylic acid.
6
Dependent← claim 1InP
The preparation method according to claim 1, wherein the high temperature treatment has a temperature within 150-300° C.
7
IndependentInPM-(O-C≡P)nZn precursorInP
A preparation method of a near-infrared InP nanocrys-tal, comprising the following steps: S1, obtaining a first solution system comprising an In precursor and an optional Zn precursor, and a second solution system comprising M-(O—C≡P)n, as a P precursor, wherein M is element Na, Li, K, Zn or Ga; S2, mixing the first solution system with the second solution system for reaction at a predetermined tem-perature to obtain the near-infrared InP nanocrystal; wherein the predetermined temperature has a range of 180-320° C., the first solution system comprises the In precursor, the optional Zn precursor and a first organic solvent dispersing the In precursor; and the second solution system comprises the P precursor and a second organic solvent dispersing the P precursor; the first organic solvent is different from the second organic solvent; and the second organic solvent has a boiling point lower than the predetermined temperature.
8
Dependent← claim 7
The preparation method according to claim 7, wherein the second organic solvent has a boiling point at least 30° C. lower than the predetermined temperature.
9
Dependent← claim 7
The preparation method according to claim 7, wherein the second organic solvent has a boiling point lower than or equal to 150° C.
The preparation method according to claim 7, wherein the In precursor is an indium halide; the first organic solvent is at least one of saturated or unsaturated amines having a carbon number not lower than 6, or carboxylic acids; and/or, the first solution system further comprises the Zn precursor; and/or, the shell of the nanocrystal comprises at least one of ZnS, ZnSe, and ZnSeS.
11
Dependent← claim 7InP
The preparation method according to claim 7, wherein the synthetic method further comprises a step S3, adding a precursor substance demanded for the synthesis of a shell of the nanocrystal to the reaction system of the S₂ step, and forming a shell on a surface of the near-infrared InP nanoc-rystal, so that the near-infrared InP nanocrystal has a fluo-rescence emission peak within 700-900 nm.
12
Dependent← claim 7
The preparation method according to claim 7, wherein the second organic solvent has a boiling point of 60-150° C.; and/or, the second organic solvent comprises at least one of benzene, methylbenzene, cyclohexane, n-hexane, n-heptane, normal octane, tetrahydrofuran and chloroform.
13
IndependentInPM-(O-C≡P)nInP
A preparation method of an red-emitting InP nanoc-rystal, comprising steps of: S1, mixing the In precursor and P precursor M-(O— C≡P)n, with an organic solvent for reaction at a first temperature, and thermally insulating for a period of time to obtain an InP nanocrystal core solution, wherein M is element Na, Li, K, Zn or Ga; S2, rapidly heating the InP nanocrystal core solution up to a second tem-perature and thermally insulating for a period of time; S3, adding a precusor substance demanded for the synthesis of a shell of the nanocrystal to the reaction system of the S₂ step to obtain the red-emitting InP nanocrystal, wherein the red-emitting InP nanocrystal has a fluorescence emission peak within 580-670 nm.
14
Dependent← claim 13
The preparation method according to claim 13, wherein the first temperature ranges from 110-160° C;and/or, the second temperature ranges from 280-340° C.
15
Dependent← claim 13
The preparation method according to claim 13, wherein in the S2, the InP nanocrystal core solution is rapidly heated up to the second temperature, keeping for at least 10 min.
16
Dependent← claim 13Zn precursorZnSZnSeZnSeS
The preparation method according to claim 13, wherein the organic solvent is selected from at least one of saturated or unsaturated amines having a carbon number not lower than 6, or carboxylic acids; and/or, the InP nanocrystal core solution optionally comprises a first Zn precursor, and the first Zn precursor is selected from a Zn halide; and/or, the shell of the nanocrystal comprises at least one of ZnS, ZnSe, and ZnSeS.
17
IndependentInPM-(O-C≡P)nInP
A preparation method of a cyan-emitting InP nanoc-rystal, comprising the following steps: S1, mixing the In precursor and P precursor M-(O— C≡P)n, with an organic solvent for reaction at a first temperature to obtain an InP nanocrystal core solution, wherein M is element Na, Li, K, Zn or Ga; S2, adding a cationic precursor to the InP nanocrystal core solution to form a first mixed solution at the first temperature; S3, adding a anionic precursor to the first mixed solution; wherein, the cationic precursor is reacted with the anionic precursor to coat a shell on the InP nanoc-rystal core, thus obtaining the cyan-emitting InP nanoc-rystal; the cyan-emitting InP nanocrystal has a fluores-cence emission peak within 460-500 nm; and wherein, B₂ the second temperature is greater than the first tem-perature.
18
Dependent← claim 17
The preparation method according to claim 17, wherein the first temperature ranges from 110-160° C;and/or, the second temperature ranges from 160-240° C.
19
Dependent← claim 17Zn precursor
The preparation method according to claim 17, wherein the organic solvent is selected from at least one of saturated or unsaturated amines having a carbon number not lower than 6, or carboxylic acids; and/or, the InP nanocrystal core solution optionally comprises a first Zn precursor, and the first Zn precursor is selected from a Zn halide; and/or, a ratio of the Zn cationic precursor in the step S₂ to the In precursor in the step S₁ is (8-40):1 according to a molar ratio; and/or, the cationic precursor is a second Zn precursor, and the second Zn precursor is selected from zinc carboxylate, or an organic zinc reagent; and/or, the anionic precursor is at least one of an S precursor and Se precursor. ∗ ∗ ∗ ∗ ∗
Materials
Materials described outside the worked examples.
InP nanocrystal
InP
Synthesis Product
M-(O—C≡P)n phosphorus precursor
M-(O-C≡P)n
Phosphorus Precursor
Zn precursor
Process steps
Additional fabrication and treatment steps described in the patent.
1
Colloidal Nanocrystal Synthesis
Step 1
Temperature
150, 340°C
Process details
method:high temperature treatment
solvent:
Characterization
Measurements and analyses referenced in the patent, with their drawing references.
tem
TEM
FIG. 2 shows a transmission electron microscopy (TEM) of a nanocrystal in example 15;
method:mixing two-solution systems at predetermined temperature; optional shell coating (S₃)
precursors:In precursor, M-(O-C≡P)n as P precursor, optional Zn precursor
first solvent:first organic solvent (amine or carboxylic acid, C>=6)
second solvent:second organic solvent (boiling point < predetermined temperature; 60-150°C; e.g., benzene, methylbenzene, cyclohexane, n-hexane, n-heptane, normal octane, tetrahydrofuran, chloroform)
shell materials:ZnS, ZnSe, ZnSeS
emission peak nm:700-900
temperature c max:150
temperature c min:60
Materials:InP
3
Colloidal Nanocrystal Synthesis
Step 3
Temperature
110, 160, 280, 340°C
Duration
10 min
Process details
method:low-temperature nucleation (S1: 110-160°C), rapid heating to second temperature (S2: 280-340°C, >=10 min), shell coating (S₃)
solvent:saturated or unsaturated amines (C>=6) or carboxylic acids
precursors:In precursor, M-(O-C≡P)n as P precursor, optional Zn halide precursor
fwhm claimed nm:<=50
shell materials:ZnS, ZnSe, ZnSeS
emission peak nm:580-670
temperature c max:160
temperature c min:110
quantum yield claimed pct:>80
temperature c lower bound:80
temperature c upper bound:50
Materials:InP
4
Colloidal Nanocrystal Synthesis
Step 4
Temperature
110, 160, 160, 240°C
Process details
method:S1: reaction at first temperature (110-160°C); S2: add cationic precursor (second Zn precursor: zinc carboxylate or organic zinc) at first temperature; S3: add anionic precursor (S or Se precursor) at second temperature (160-240°C) to coat shell
solvent:saturated or unsaturated amines (C>=6) or carboxylic acids
precursors:In precursor, M-(O-C≡P)n as P precursor, optional Zn halide precursor (first Zn precursor)
method:mixing two-solution systems at predetermined temperature; optional shell coating (S₃)
precursors:In precursor, M-(O-C≡P)n as P precursor, optional Zn precursor
first solvent:first organic solvent (amine or carboxylic acid, C>=6)
second solvent:second organic solvent (boiling point < predetermined temperature; 60-150°C; e.g., benzene, methylbenzene, cyclohexane, n-hexane, n-heptane, normal octane, tetrahydrofuran, chloroform)
shell materials:ZnS, ZnSe, ZnSeS
emission peak nm:700-900
temperature c max:150
temperature c min:60
Materials:InP
3
Colloidal Nanocrystal Synthesis
Step 3
Temperature
110, 160, 280, 340°C
Duration
10 min
Process details
method:low-temperature nucleation (S1: 110-160°C), rapid heating to second temperature (S2: 280-340°C, >=10 min), shell coating (S₃)
solvent:saturated or unsaturated amines (C>=6) or carboxylic acids
precursors:In precursor, M-(O-C≡P)n as P precursor, optional Zn halide precursor
fwhm claimed nm:<=50
shell materials:ZnS, ZnSe, ZnSeS
emission peak nm:580-670
temperature c max:160
temperature c min:110
quantum yield claimed pct:>80
temperature c lower bound:80
temperature c upper bound:50
Materials:InP
4
Colloidal Nanocrystal Synthesis
Step 4
Temperature
110, 160, 160, 240°C
Process details
method:S1: reaction at first temperature (110-160°C); S2: add cationic precursor (second Zn precursor: zinc carboxylate or organic zinc) at first temperature; S3: add anionic precursor (S or Se precursor) at second temperature (160-240°C) to coat shell
solvent:saturated or unsaturated amines (C>=6) or carboxylic acids
precursors:In precursor, M-(O-C≡P)n as P precursor, optional Zn halide precursor (first Zn precursor)
method:mixing two-solution systems at predetermined temperature; optional shell coating (S₃)
precursors:In precursor, M-(O-C≡P)n as P precursor, optional Zn precursor
first solvent:first organic solvent (amine or carboxylic acid, C>=6)
second solvent:second organic solvent (boiling point < predetermined temperature; 60-150°C; e.g., benzene, methylbenzene, cyclohexane, n-hexane, n-heptane, normal octane, tetrahydrofuran, chloroform)
shell materials:ZnS, ZnSe, ZnSeS
emission peak nm:700-900
temperature c max:150
temperature c min:60
Materials:InP
3
Colloidal Nanocrystal Synthesis
Step 3
Temperature
110, 160, 280, 340°C
Duration
10 min
Process details
method:low-temperature nucleation (S1: 110-160°C), rapid heating to second temperature (S2: 280-340°C, >=10 min), shell coating (S₃)
solvent:saturated or unsaturated amines (C>=6) or carboxylic acids
precursors:In precursor, M-(O-C≡P)n as P precursor, optional Zn halide precursor
fwhm claimed nm:<=50
shell materials:ZnS, ZnSe, ZnSeS
emission peak nm:580-670
temperature c max:160
temperature c min:110
quantum yield claimed pct:>80
temperature c lower bound:80
temperature c upper bound:50
Materials:InP
4
Colloidal Nanocrystal Synthesis
Step 4
Temperature
110, 160, 160, 240°C
Process details
method:S1: reaction at first temperature (110-160°C); S2: add cationic precursor (second Zn precursor: zinc carboxylate or organic zinc) at first temperature; S3: add anionic precursor (S or Se precursor) at second temperature (160-240°C) to coat shell
solvent:saturated or unsaturated amines (C>=6) or carboxylic acids
precursors:In precursor, M-(O-C≡P)n as P precursor, optional Zn halide precursor (first Zn precursor)
method:mixing two-solution systems at predetermined temperature; optional shell coating (S₃)
precursors:In precursor, M-(O-C≡P)n as P precursor, optional Zn precursor
first solvent:first organic solvent (amine or carboxylic acid, C>=6)
second solvent:second organic solvent (boiling point < predetermined temperature; 60-150°C; e.g., benzene, methylbenzene, cyclohexane, n-hexane, n-heptane, normal octane, tetrahydrofuran, chloroform)
shell materials:ZnS, ZnSe, ZnSeS
emission peak nm:700-900
temperature c max:150
temperature c min:60
Materials:InP
3
Colloidal Nanocrystal Synthesis
Step 3
Temperature
110, 160, 280, 340°C
Duration
10 min
Process details
method:low-temperature nucleation (S1: 110-160°C), rapid heating to second temperature (S2: 280-340°C, >=10 min), shell coating (S₃)
solvent:saturated or unsaturated amines (C>=6) or carboxylic acids
precursors:In precursor, M-(O-C≡P)n as P precursor, optional Zn halide precursor
fwhm claimed nm:<=50
shell materials:ZnS, ZnSe, ZnSeS
emission peak nm:580-670
temperature c max:160
temperature c min:110
quantum yield claimed pct:>80
temperature c lower bound:80
temperature c upper bound:50
Materials:InP
4
Colloidal Nanocrystal Synthesis
Step 4
Temperature
110, 160, 160, 240°C
Process details
method:S1: reaction at first temperature (110-160°C); S2: add cationic precursor (second Zn precursor: zinc carboxylate or organic zinc) at first temperature; S3: add anionic precursor (S or Se precursor) at second temperature (160-240°C) to coat shell
solvent:saturated or unsaturated amines (C>=6) or carboxylic acids
precursors:In precursor, M-(O-C≡P)n as P precursor, optional Zn halide precursor (first Zn precursor)