# US 9,518,216 B2 · Manganese-doped magnesium stannate luminescent material and preparation method therefor

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- Number: US 9,518,216 B2
- Document ID: US9518216B2
- Status: Granted
- Kind: B2
- Application number: 14/399,732
- Filed: 2012-05-08
- Published: 2015-03-26
- Granted: 2016-12-13
- Earliest claimed: 2012-05-08
- Assignees: Ocean's King Lighting Science & Technology Co., Ltd.
- Applicants: Mingjie Zhou; Rong Wang; Guitang Chen
- Inventors: Mingjie Zhou; Rong Wang; Guitang Chen
- Web page: https://patentgrep.com/patent/US9518216B2

## CPC

- C09K 11/025: {non-luminescent particle coatings or suspension media}
- C09K 11/66: containing germanium, tin or lead
- C09K 11/661: {Chalcogenides}
- C09K 11/663: {with alkaline earth metals}
- C09K 11/7731: {with alkaline earth metals}
- C09K 11/87: containing platina group metals
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE

## Abstract

A manganese-doped magnesium stannate luminescent material, which has a molecular formula of: Mg2-xSnO4:Mnx@SnO2@My, where @ is a coating, where Mg2-xSnO4:Mnx is an outer shell layer, where SnO2 is an intermediate layer shell, where M is an inner core, where M is a metal nanoparticle, where M is at least one selected among Ag, Au, Pt, Pd, and Cu, where the value of x is 0<x≦0.05, where y is the molar ratio between M and Sn, and where the value of y is 0<y≦1×10−2. The manganese-doped magnesium stannate luminescent material is a core-shell structure luminescent material, has a high internal quantum efficiency, great luminescent intensity, and the advantages of great stability and great luminescent properties. A method for preparing the manganese-doped magnesium stannate luminescent material has simple processes, low equipment requirements, and no pollution, is easy to control and applicable for industrial production, and has a broad application prospect.

## Claims

### Claim 1

A manganese-doped magnesium stannate luminescent material having a chemical formula of Mg2-xSnO4:Mnx@SnO2@My, where @ denotes coating; Mg2-xSnO4:Mnx is outer shell layer; SnO2 is intermediate layer shell; M is inner core; M is metal nanoparticle; M is at least one of Ag, Au, Pt, Pd and Cu; x is in a range of 0<x≦0.05; y is molar ratio of M to the amount of tin in SnO2; y is in a range of 0<y≦1×10−2.

### Claim 2 (depends on 1)

The manganese-doped magnesium stannate luminescent material of claim 1, wherein x is in a range of 0.002≦x≦0.008, y is in a range of 1×10−5<y≦1×10−3.

### Claim 3

A method for preparing manganese-doped magnesium stannate luminescent material, comprising:
(1) mixing solution of metal salt, additive with reducing agent, then reacting to produce metal nanoparticles colloid, the solution of metal salt is at least one solution of Ag salt, Au salt, Pt salt, Pd salt and Cu salt; the additive is at least one of polyvinylpyrrolidone, sodium citrate, cetyl trimethyl ammonium bromide, sodium dodecyl sulfate and sodium dodecyl sulfonate;
(2) adding the metal nanoparticles colloid into solvent and stirring to produce solution containing surface-treated metal nanoparticles; the solvent is selected from the group consisting of aqueous solution of polyvinylpyrrolidone, polyvinyl alcohol, polypropylene glycol and cetyl trimethyl ammonium bromide;
(3) adjusting pH value of the solution containing surface-treated metal nanoparticles to 10-11, heating in a water bath at a temperature of 50° C.-70° C., adding Na2SnO3 while stirring, then separating and drying to obtain SnO2 powder coating metal nanoparticles;
(4) weighing compound used as source of Mg, compound used as source of Mn and the SnO2 powder coating metal nanoparticles according to stoichiometric ratio, mixing well, elevating the temperature to 800° C.-1200° C. and calcining for 2-12 h, reducing at a temperature in the range of 1000° C.-1400° C. for 0.5-6 h, cooling with furnace to room temperature, obtaining manganese-doped magnesium stannate luminescent material.

### Claim 4 (depends on 3)

The method for preparing manganese-doped magnesium stannate luminescent material of claim 3, wherein concentration of the solution of metal salt is in a range of 1×10−3 mol/L-5×10−2 mol/L.

### Claim 5 (depends on 3)

The method for preparing manganese-doped magnesium stannate luminescent material of claim 3, wherein the additive is added in an amount sufficient to adjust the concentration of additive in obtained metal nanoparticles colloid to 1×10−4 g/mL-5×10−2 g/mL.

### Claim 6 (depends on 3)

The method for preparing manganese-doped magnesium stannate luminescent material of claim 3, wherein the reducing agent is at least one of hydrazine hydrate, ascorbic acid, sodium citrate and sodium borohydride; reducing agent is an aqueous solution having a concentration in a range of 1×10−4 mol/L-1 mol/L; molar ratio of reducing agent to metal ion is in a range of 3.6:1-18:1.

### Claim 7 (depends on 3)

The method for preparing manganese-doped magnesium stannate luminescent material of claim 3, wherein the step (3) comprises: adjusting pH value of solution containing surface-treated metal nanoparticles to 10.5 by adding NaOH solution, heating in a water bath at 60° C., rapidly adding Na2SnO3 while stirring, then separating and drying to obtain SnO2 powder coating metal nanoparticles.

### Claim 8 (depends on 3)

The method for preparing manganese-doped magnesium stannate luminescent material of claim 3, wherein the compound used as source of Mg is selected from oxide of Mg, carbonate of Mg, acetate of Mg and oxalate of Mg.

### Claim 9 (depends on 3)

The method for preparing manganese-doped magnesium stannate luminescent material of claim 3, wherein the compound used as source of Mn is selected from oxide of Mn, carbonate of Mn, acetate of Mn and oxalate of Mn.

### Claim 10 (depends on 3)

The method for preparing manganese-doped magnesium stannate luminescent material of claim 3, wherein the step of reducing is conducted in reducing atmosphere consisting of at least one of mixed gases of N2 and H2, CO, and H2.