CN1236011C - Method for preparing phosphor powder in high-luminance - Google Patents
Method for preparing phosphor powder in high-luminance Download PDFInfo
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- CN1236011C CN1236011C CN 200410026054 CN200410026054A CN1236011C CN 1236011 C CN1236011 C CN 1236011C CN 200410026054 CN200410026054 CN 200410026054 CN 200410026054 A CN200410026054 A CN 200410026054A CN 1236011 C CN1236011 C CN 1236011C
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- Prior art keywords
- substrate material
- zinc sulphide
- quartz
- sulphur
- aluminium sesquioxide
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Abstract
The present invention relates to a preparation method of phosphor powder with high luminance, which comprises the following steps: firstly, preparing a substrate material by mixing 40 to 200 shares of zinc sulfide with 0.0235 to 0.0881% of cupric nitrate, 0 to 0.012% of aurum, 0.01 to 0.20% of bismuth iodide, 0.01 to 0.20% of potassium iodide, 0.01 to 0.2% of ammonium iodide, 0.04 to 0.30% of strontium bromide, 1 to 4% of sulphur and 1 to 3% of ammonium bicarbonate measured by zinc sulfide; adding 0.007 to 0.33% of aluminium oxide in a gamma crystal form measured by the zinc sulfide to the substrate material and uniformly stirring the aluminium oxide and the substrate material; finally, adding a quartz boat loaded with 5 to 30% of sulphur and 5 to 30% of active carbon measured by the zinc sulfide to the substrate material containing the aluminium oxide, and putting the mixture in a quartz container which is provided with a quartz cover; putting the quartz boat on the surface of the substrate material; afterwards, sintering the mixture at 940 to 990 DEG C for 60 to 180 minutes in a tunnel type electricity furnace under the protection of nitrogen. Because the present invention adopts a method of directly adding the highly active Al2O3, so Al<3+> easily enters lattices of ZnS, and the luminance of the phosphor powder is improved consequently.
Description
Technical field
The present invention relates to a kind of preparation method of cathode-ray tube phosphor of high brightness.
Background technology
Cathode-ray tube ZnS: CuAL or ZnS: the green light-emitting fluorescent powder that the CuALAu formula is represented, its contained Al coactivator when introducing the Al coactivator now, adopt traditional Al (NO to its brightness decisive role always
3)
3Introduce with the form that the ZnS wet-mixed makes, the product that this method makes is called Al kind powder, and (Al kind powder, this processing method complexity must be Al (NO
3)
3Make a certain proportion of solution earlier, then by a certain percentage the Al (NO for preparing
3)
3Solution and ZnS powder and pure water are in harmonious proportion evenly, are placed in the fine aluminium drying tray by a certain amount of, and at 140 ℃ electric drying apparatus inner drying, the nylon screen with certain order number sieves then, mixes to get final product), be converted into Al
2S
3, finally make Al
3+Enter in the ZnS lattice; And Al (NO
3)
3Under sintering temperature, be decomposed into Al
2O
3, its stable in properties is because solid Al
2O
3Have three kinds of crystal formations to exist, be respectively α, β and γ, because their surface-area difference, they are active different, determine them that very big difference is arranged, general γ-Al
2O
3Active maximum, and α-Al
2O
3Active minimum; In addition because Al
2O
3Changeing crystal formation at 400-700 ℃ is γ-Al
2O
3, changeing crystal formation about 1200 ℃ greatly is final α-Al
2O
3, and sintering temperature is generally 960-990 ℃, so with traditional Al (NO
3)
3Form is introduced, Al
2O
3Trend towards a crystal formation, its character is than γ-Al
2O
3Stable, just be not easy to make Al
3+Enter in the ZnS lattice, thus unfavorable to the height of fluorescent material.Totally, there is shortcoming in prior art: the Al coactivator is introduced complex manufacturing technology, cost of manufacture height, fluorescent material brightness shortcoming.
Summary of the invention
The object of the present invention is to provide a kind of preparation simple, and can improve the preparation method of the phosphor of high brightness of picture tube brightness.
For achieving the above object, the preparation method that the present invention adopts is: at first the potassiumiodide of cupric nitrate, 0～gold of 0.12 ‰ of 0.235～0.881 ‰ of 40～200 parts zinc sulphide and zinc sulphide quality, 0.01～0.20% bismuth iodide, 0.01～.20%, 0.01～0.20% ammonium iodide, 0.04～0.30% strontium bromide, 1～4% sulphur and 1～3% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of the γ crystal formation of 0.07 of zinc sulphide quality～0.3 ‰ is added in the substrate material and stir; The quartz boat that 5～30% sulphur of zinc sulphide quality and 5～30% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 940～990 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 60～180 minutes.
Because the present invention adopts the highly active Al of direct adding
2O
3Method, make Al
3+Easier entering in the ZnS lattice, thereby the brightness that has improved fluorescent material.
Embodiment
Embodiment 1: at first 0.881 ‰ cupric nitrate of 40 parts zinc sulphide and zinc sulphide quality, 0.01% bismuth iodide, 0.01% potassiumiodide, 0.1% ammonium iodide, 0.3% strontium bromide, 4% sulphur and 3% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.3 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; Specific surface area 〉=the 120m of the aluminium sesquioxide of this γ crystal formation
2/ g, size-grade distribution d50=3-8 μ m, loose density are 0.35-0.50g/cm
3, purity 〉=99.995%, ICP foreign matter content Fe≤8ppm; The quartz boat that 5% sulphur of zinc sulphide quality and 30% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 940 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 180 minutes.
Embodiment 2: at first 0.235 ‰ cupric nitrate of 120 parts zinc sulphide and zinc sulphide quality, 0.12 ‰ gold, 0.2% bismuth iodide, 0.1% potassiumiodide, 0.09% ammonium iodide, 0.04% strontium bromide, 1% sulphur and 2% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.07 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 30% sulphur of zinc sulphide quality and 5% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 990 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 60 minutes.
Embodiment 3: at first 0.35 ‰ cupric nitrate of 80 parts zinc sulphide and zinc sulphide quality, 0.05 ‰ gold, 0.05% bismuth iodide, 0.12% potassiumiodide, 0.01% ammonium iodide, 0.24% strontium bromide, 3% sulphur and 1% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.09 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 25% sulphur of zinc sulphide quality and 12% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 960 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 120 minutes.
Embodiment 4: at first 0.6 ‰ cupric nitrate of 100 parts zinc sulphide and zinc sulphide quality, 0.1 ‰ gold, 0.1% bismuth iodide, 0.09% potassiumiodide, 0.17% ammonium iodide, 0.08% strontium bromide, 2% sulphur and 1.5% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.2 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 10% sulphur of zinc sulphide quality and 23% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 980 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 150 minutes.
Embodiment 5: at first 0.42 ‰ cupric nitrate of 60 parts zinc sulphide and zinc sulphide quality, 0.08 ‰ gold, 0.09% bismuth iodide, 0.2% potassiumiodide, 0.2% ammonium iodide, 0.1% strontium bromide, 1.5% sulphur and 2.6% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.1 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 8% sulphur of zinc sulphide quality and 19% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 950 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 93 minutes.
Embodiment 6: at first 0.78 ‰ cupric nitrate of 75 parts zinc sulphide and zinc sulphide quality, 0.17% bismuth iodide, 0.05% potassiumiodide, 0.12% ammonium iodide, 0.25% strontium bromide, 2.3% sulphur and 1.9% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.15 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 17% sulphur of zinc sulphide quality and 25% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 970 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 72 minutes.
Embodiment 7: at first 0.55 ‰ cupric nitrate of 53 parts zinc sulphide and zinc sulphide quality, 0.04 ‰ gold, 0.12% bismuth iodide, 0.17% potassiumiodide, 0.05% ammonium iodide, 0.14% strontium bromide, 3.8% sulphur and 2.3% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.24 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 26% sulphur of zinc sulphide quality and 8% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 965 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 169 minutes.
Claims (8)
1, a kind of preparation method of phosphor of high brightness is characterized in that:
1) at first cupric nitrate, 0～gold of 0.12 ‰ of 0.235～0.881 ‰ of 40～200 parts zinc sulphide and zinc sulphide quality, 0.01～0.20% bismuth iodide, 0.01～0.20% potassiumiodide, 0.01～0.20% ammonium iodide, 0.04～0.30% strontium bromide, 1～4% sulphur and 1～3% bicarbonate of ammonia are mixed and made into substrate material;
2) aluminium sesquioxide of the γ crystal formation of 0.07 of zinc sulphide quality～0.3 ‰ is added in the substrate material stir again;
3) quartz boat that 5～30% sulphur of zinc sulphide quality and 5～30% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 940～990 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 60～180 minutes.
2, the preparation method of phosphor of high brightness according to claim 1 is characterized in that: at first 0.881 ‰ cupric nitrate of 40 parts zinc sulphide and zinc sulphide quality, 0.01% bismuth iodide, 0.01% potassiumiodide, 0.1% ammonium iodide, 0.3% strontium bromide, 4% sulphur and 3% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.3 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 5% sulphur of zinc sulphide quality and 30% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 940 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 180 minutes.
3, the preparation method of phosphor of high brightness according to claim 1 is characterized in that: at first 0.235 ‰ cupric nitrate of 120 parts zinc sulphide and zinc sulphide quality, 0.12 ‰ gold, 0.2% bismuth iodide, 0.1% potassiumiodide, 0.09% ammonium iodide, 0.04% strontium bromide, 1% sulphur and 2% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.07 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 30% sulphur of zinc sulphide quality and 5% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 990 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 60 minutes.
4, the preparation method of phosphor of high brightness according to claim 1 is characterized in that: at first 0.35 ‰ cupric nitrate of 80 parts zinc sulphide and zinc sulphide quality, 0.05 ‰ gold, 0.05% bismuth iodide, 0.12% potassiumiodide, 0.01% ammonium iodide, 0.24% strontium bromide, 3% sulphur and 1% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.09 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 25% sulphur of zinc sulphide quality and 12% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 960 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 120 minutes.
5, the preparation method of phosphor of high brightness according to claim 1 is characterized in that: at first 0.6 ‰ cupric nitrate of 100 parts zinc sulphide and zinc sulphide quality, 0.1 ‰ gold, 0.1% bismuth iodide, 0.09% potassiumiodide, 0.17% ammonium iodide, 0.08% strontium bromide, 2% sulphur and 1.5% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.2 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 10% sulphur of zinc sulphide quality and 23% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 980 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 150 minutes.
6, the preparation method of phosphor of high brightness according to claim 1 is characterized in that: at first 0.42 ‰ cupric nitrate of 60 parts zinc sulphide and zinc sulphide quality, 0.08 ‰ gold, 0.09% bismuth iodide, 0.2% potassiumiodide, 0.2% ammonium iodide, 0.1% strontium bromide, 1.5% sulphur and 2.6% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.1 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 8% sulphur of zinc sulphide quality and 19% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 950 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 93 minutes.
7, the preparation method of phosphor of high brightness according to claim 1 is characterized in that: at first 0.78 ‰ cupric nitrate of 75 parts zinc sulphide and zinc sulphide quality, 0.17% bismuth iodide, 0.05% potassiumiodide, 0.12% ammonium iodide, 0.25% strontium bromide, 2.3% sulphur and 1.9% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.15 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 17% sulphur of zinc sulphide quality and 25% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 970 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 72 minutes.
8, the preparation method of phosphor of high brightness according to claim 1 is characterized in that: at first 0.55 ‰ cupric nitrate of 53 parts zinc sulphide and zinc sulphide quality, 0.04 ‰ gold, 0.12% bismuth iodide, 0.17% potassiumiodide, 0.05% ammonium iodide, 0.14% strontium bromide, 3.8% sulphur and 2.3% bicarbonate of ammonia are mixed and made into substrate material; Again the aluminium sesquioxide of 0.24 ‰ γ crystal formation of zinc sulphide quality is added in the substrate material and stir; The quartz boat that 26% sulphur of zinc sulphide quality and 8% gac will be housed at last has the substrate material of aluminium sesquioxide together to put into the quartz container that has quartz cover with adding; and quartz boat got final product at 965 ℃ of sintering in the electric stove of the tunnel like that nitrogen protection is arranged on the substrate material surface afterwards in 169 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410026054 CN1236011C (en) | 2004-04-19 | 2004-04-19 | Method for preparing phosphor powder in high-luminance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410026054 CN1236011C (en) | 2004-04-19 | 2004-04-19 | Method for preparing phosphor powder in high-luminance |
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| Publication Number | Publication Date |
|---|---|
| CN1563268A CN1563268A (en) | 2005-01-12 |
| CN1236011C true CN1236011C (en) | 2006-01-11 |
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|---|---|---|---|
| CN 200410026054 Expired - Fee Related CN1236011C (en) | 2004-04-19 | 2004-04-19 | Method for preparing phosphor powder in high-luminance |
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| CN (1) | CN1236011C (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE102013114496A1 (en) * | 2013-12-19 | 2015-06-25 | Bundesdruckerei Gmbh | Zinc sulfide phosphor with photo and electroluminescent behavior, process for its preparation and security document, security feature and method for its detection |
| CN103992793A (en) * | 2014-05-04 | 2014-08-20 | 徐州工程学院 | Preparation method for high-chroma green phosphor |
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| CN1563268A (en) | 2005-01-12 |
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| ASS | Succession or assignment of patent right |
Owner name: IRICO GROUP ELECTRONICS CO., LTD. Free format text: FORMER OWNER: CAIHONG COLOUR KINESCOPE GENERAL FACTORY Effective date: 20041126 |
|
| C06 | Publication | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| PB01 | Publication | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20041126 Address after: No. 1 Rainbow Road, Shaanxi, Xianyang Applicant after: IRICO Group Electronics Co., Ltd. Address before: No. 1 Rainbow Road, Shaanxi, Xianyang Applicant before: Caihong Color CRT General Factory |
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| C10 | Entry into substantive examination | ||
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| C14 | Grant of patent or utility model | ||
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20060111 Termination date: 20130419 |