CN102418085A - Micronano-scale powder protective layer wrapping device and method - Google Patents
Micronano-scale powder protective layer wrapping device and method Download PDFInfo
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- CN102418085A CN102418085A CN2011104193584A CN201110419358A CN102418085A CN 102418085 A CN102418085 A CN 102418085A CN 2011104193584 A CN2011104193584 A CN 2011104193584A CN 201110419358 A CN201110419358 A CN 201110419358A CN 102418085 A CN102418085 A CN 102418085A
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Abstract
The invention provides a micronano-scale powder protective layer wrapping device and a micronano-scale powder protective layer wrapping method. The device comprises a vacuum system, a reaction cavity system, a precursor pulse system, a heating system, a carrier gas transmission system and a control system, wherein the precursor pulse system is connected with the reaction cavity system; the reaction cavity system is connected with the vacuum system; a connecting channel of the precursor pulse system and the reaction cavity system is connected with the carrier gas transmission system; and the heating system comprises heating devices arranged on the system devices. The micronano-scale powder protective layer wrapping method comprises the following steps of: wrapping the micronano-scale powder in the vacuum reaction cavity by using a protective layer and an atomic layer deposition (ALD) technology at a certain temperature; allowing a precursor source material to enter the reaction cavity system through carrier gas alternation by using a pulse actuator, wherein a micro-scale hole is formed on the end face of the inner cavity accommodating the powder; and cleaning the redundant precursor source material and reaction byproducts by using the carrier gas so as to obtain the required micronano-scale powder wrapped by the protective layer.
Description
Technical field
The present invention relates to a kind of micro/nano-scale powder resist Wrap device and method, belong to powder deposition apparatus and technical field.
Background technology
The micro-nano-scale powder is because particle diameter is little; The surface key is many; Therefore usually show the excellent specific property that is different from massive material; But simultaneously, it also has easy reunion, a series of shortcomings such as oxidized, character instability easily, becomes a kind of important method that solves these a series of shortcomings of micro/nano-scale powder in the method for micro/nano-scale powder surface packing protective layer.Have the stability that chemically inert resist can not only increase nanoparticle at the powder surface parcel, but also can make the powder granule of the micro/nano-scale after the coating have certain functional type.But often thickness is thicker for the resist that the packaging method of common micro nano powder (like liquid phase method) forms at particle surface, and the variable thickness of different positions causes, and has reduced the use properties of material to a great extent.
Ald (ALD) technology be a kind of can be with material with the monatomic form membrane method that is plated in substrate surface in layer, so it can carry out packing protective layer to the micro-nano-scale powder effectively.Utilized technique for atomic layer deposition on the large size sample, to carry out plated film in the past more; And it is little for the powder granule of micro/nano-scale owing to its particle; In vacuum cavity, be easy to taken away by high speed vacuum pump; Therefore need prevent the protection taken away to particle, but solve the problem that the precursor source material effectively touches the powder granule surface simultaneously again.
Summary of the invention
The technical problem that the present invention will solve is to overcome existing defective; A kind of micro/nano-scale powder resist Wrap device and method are provided; Can make each particle surface resist deposit thickness even, consistency of thickness on the sealer three-dimensional, and can prevent that powder granule from being taken away.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
A kind of micro/nano-scale powder resist Wrap device; Comprise vacuum system, reaction cavity system, presoma pulse system, heating system, carrier gas delivery system, system; Presoma pulse system ligation cavity system; The reaction cavity system connects vacuum system, on the connecting path of presoma pulse system and reaction cavity system, is connected with the carrier gas delivery system, and heating system comprises the heating unit that is arranged on the aforementioned system device.
Further, the presoma pulse system comprises many parallel branches, and two or more different precursor source material are provided respectively, and its major parts comprises pulse performer and source material storage steel bottle, the manual seal valve of configuration between pulse performer and source material storage steel bottle.
Further, the pulse performer is the normal closed gate that the minimum opening time can reach 10ms, and a plurality of pulse performer are alternately opened, and the source interior precursor source material of material storage steel bottle alternately gets into the reaction cavity internal system.
Further, the precursor source material is any one of liquid source or Solid State Source with higher saturated vapor pressure.
Further, the reaction cavity system is inside and outside two cavity design, and external cavity is made up of hinged two portions up and down; Top is can be around the lid of hinge opening and closing; Cover handle is installed, the external cavity both sides are respectively arranged with inlet mouth and air outlet, and inlet mouth connects presoma pulse system and carrier gas delivery system; The air outlet connects vacuum system, and the external cavity set inside has ir heaters; Internal cavity is the powdered reaction device, and inside is evenly distributed with strip mixing tank vertically, and two bottom surfaces are stainless (steel) wire, and one of them bottom surface is detachable bottom surface, and two bottom surface arranged outside have rotating shaft, extend to outside the external cavity, are connected with drive unit.
Further, inside and outside two cavitys of reaction cavity system can preferably two-layer right cylinder design.
Further, heating system is that reaction cavity system, pipeline, source material storage steel bottle and pulse performer heat.
Further, system is used to control the open and close of vacuum system, time and cleaning time, cycle index and the temperature controlled setting of source material pulse.
A kind of micro/nano-scale powder resist packaging method; At a certain temperature; Adopt ALD technology powder to micro/nano-scale in the vacuum reaction cavity to carry out the resist parcel; Reaction cavity is inside and outside two cavitys, and the inner chamber body of splendid attire powder has micrometer grade hole at end face, makes the precursor source material alternately get into the reaction cavity system through carrier gas through the pulse performer; And utilize unnecessary precursor source material and the byproduct of reaction of carrier gas cleaning, thereby obtain required micro/nano-scale powder with resist parcel.
Further, the temperature of reaction cavity system is a room temperature to 300 ℃.
Description of drawings
Accompanying drawing is used to provide further understanding of the present invention, and constitutes the part of specification sheets, is used to explain the present invention with embodiments of the invention, is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the structural representation of a kind of micro/nano-scale powder of the present invention resist Wrap device;
Fig. 2 is the main TV structure synoptic diagram of external cavity;
Fig. 3 is the plan structure synoptic diagram of external cavity;
Fig. 4 is the right TV structure synoptic diagram of external cavity;
Fig. 5 is the structural representation of powdered reaction device;
Fig. 6 is the A-A structural representation of powdered reaction device;
Fig. 7 is the B-B of powdered reaction device
/Structural representation;
Fig. 8 is the C-C of powdered reaction device
/Structural representation;
Fig. 9 is the D-D of powdered reaction device
/Structural representation.
Embodiment
Below in conjunction with accompanying drawing the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein only is used for explanation and explains the present invention, and be not used in qualification the present invention.
As shown in Figure 1; A kind of micro/nano-scale powder resist Wrap device; Comprise vacuum system, reaction cavity system, presoma pulse system, heating system, carrier gas delivery system, system; Presoma pulse system ligation cavity system, the reaction cavity system connects vacuum system, and vacuum system comprises vacuum pump 18 and vacuum open valve 17.
On the connecting path of presoma pulse system and reaction cavity system, be connected with the carrier gas delivery system, under meter 7 is installed on the carrier gas transfer line 6, heating system comprises the heating unit that is arranged on the aforementioned system device.
The presoma pulse system comprises two parallelly connected presoma branch roads 8 and 9, and two or more different precursor source material TMA and H are provided respectively
2O, its major parts comprise pulse performer 10 and source material storage steel bottle 14, the manual seal valve 12 of configuration between pulse performer 10 and source material storage steel bottle 14.
The reaction cavity system is inside and outside two cavity design, and inside and outside two cavitys can preferably two-layer right cylinder design.External cavity 1 is made up of hinged two portions up and down, and top is to cover on 19 handle 21 is installed around the lid 19 of hinge 22 foldings; The bottom is for going to the bottom 20; External cavity, 1 both sides are respectively arranged with inlet mouth 23 and air outlet 24, and inlet mouth 23 connects the total pipeline 5 of presoma pulse system and carrier gas delivery system; Air outlet 24 connects the vacuum-lines 16 of vacuum system, and the external cavity set inside has ir heaters.
Like Fig. 1,5,6,7,8, shown in 9, internal cavity is a powdered reaction device 2, and inside is evenly distributed with strip mixing tank 26 vertically; Two bottom surfaces are stainless (steel) wire 27; Mesh is 10 microns, and one of them bottom surface is detachable bottom surface, the convenient adding and the taking-up powder.Seal with sealring 28 between this bottom surface and the powdered reaction device body.Two bottom surface arranged outside have rotating shaft 29, extend to outside the external cavity 1, are connected with drive unit.
Heating system is that reaction cavity system, pipeline, source material storage steel bottle and pulse performer heat.
System is used to control the open and close of vacuum system, time and cleaning time, cycle index and the temperature controlled setting of source material pulse.
A kind of micro/nano-scale powder resist packaging method; The reaction cavity system is under 200 ℃ temperature; Adopt ALD technology powder to micro/nano-scale in the vacuum reaction cavity to carry out the resist parcel; Reaction cavity is inside and outside two cavitys, and the inner chamber body of splendid attire powder has micrometer grade hole at end face, makes the precursor source material alternately get into the reaction cavity system through carrier gas through the pulse performer; And utilize unnecessary precursor source material and the byproduct of reaction of carrier gas cleaning, thereby obtain required micro/nano-scale powder with resist parcel.
Embodiment one
Adopt said apparatus micro/nano-scale powder resist Wrap device method of use following:
Open external cavity, take out inner powdered reaction device, the powder of needs parcel is put into back sealed external cavity.The open vacuum pump, the open vacuum open valve when treating that vacuum reaches required vacuum tightness and requires (being less than or equal to 1 pa), gets into next step so that vacuum cavity is connected with vacuum pump then;
The temperature of reaction cavity system, equipment pipeline and miscellaneous part is set; It is 200 ℃ that reaction cavity internal system temperature is set; It is 120 ℃ that the pipeline temperature is set; The temperature of pulse performer is 130 ℃, and is identical with established temperature and get into next step when reaching stable (fluctuation range is less than or equal to 1 ℃) when displays temperature;
Open the manual seal valve of presoma steel cylinder and, burst length that first presoma (TMA) and second presoma (H2O) be set 10ms not all, flush time is set to 10s and 15s respectively; Cycle index is set to 100; Carrier gas flux is set to 20sccm; The beginning cyclic deposition, deposition can form the plating aluminium oxide film that thickness is about 10 nanometers at particle surface after finishing.
What should explain at last is: the above is merely the preferred embodiments of the present invention; Be not limited to the present invention; Although the present invention has been carried out detailed explanation with reference to previous embodiment; For a person skilled in the art, it still can be made amendment to the technical scheme that aforementioned each embodiment put down in writing, and perhaps part technical characterictic wherein is equal to replacement.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. micro/nano-scale powder resist Wrap device; It is characterized in that: comprise vacuum system, reaction cavity system, presoma pulse system, heating system, carrier gas delivery system, system; Presoma pulse system ligation cavity system; The reaction cavity system connects vacuum system, on the connecting path of presoma pulse system and reaction cavity system, is connected with the carrier gas delivery system, and heating system comprises the heating unit that is arranged on the aforementioned system device.
2. a kind of micro/nano-scale powder resist Wrap device as claimed in claim 1; It is characterized in that: the presoma pulse system comprises many parallel branches; Two or more different precursor source material are provided respectively; Its major parts comprises pulse performer and source material storage steel bottle, the manual seal valve of configuration between pulse performer and source material storage steel bottle.
3. a kind of micro/nano-scale powder resist Wrap device as claimed in claim 2; It is characterized in that: the pulse performer can reach the normal closed gate of 10ms for the minimum opening time; A plurality of pulse performer are alternately opened, and the precursor source material in the material storage steel bottle of source alternately gets into the reaction cavity internal system.
4. a kind of micro/nano-scale powder resist Wrap device as claimed in claim 3 is characterized in that: the precursor source material is any one of liquid source or Solid State Source with higher saturated vapor pressure.
5. a kind of micro/nano-scale powder resist Wrap device as claimed in claim 1, it is characterized in that: the reaction cavity system is inside and outside two cavity design, external cavity is made up of hinged two portions up and down; Top is can be around the lid of hinge opening and closing; Cover handle is installed, the external cavity both sides are respectively arranged with inlet mouth and air outlet, and inlet mouth connects presoma pulse system and carrier gas delivery system; The air outlet connects vacuum system, and the external cavity set inside has ir heaters; Internal cavity is the powdered reaction device, and inside is evenly distributed with strip mixing tank vertically, and two bottom surfaces are stainless (steel) wire, and one of them bottom surface is detachable bottom surface, and two bottom surface arranged outside have rotating shaft, extend to outside the external cavity, are connected with drive unit.
6. a kind of micro/nano-scale powder resist Wrap device as claimed in claim 5 is characterized in that: inside and outside two cavitys of reaction cavity system can preferably two-layer right cylinder design.
7. a kind of according to claim 1 micro/nano-scale powder resist Wrap device is characterized in that: heating system is that reaction cavity system, pipeline, source material storage steel bottle and pulse performer heat.
8. a kind of according to claim 1 micro/nano-scale powder resist Wrap device is characterized in that: system is used to control the open and close of vacuum system, time and cleaning time, cycle index and the temperature controlled setting of source material pulse.
9. micro/nano-scale powder resist packaging method; It is characterized in that: at a certain temperature; Adopt ALD technology powder to micro/nano-scale in the vacuum reaction cavity to carry out the resist parcel; Reaction cavity is inside and outside two cavitys, and the inner chamber body of splendid attire powder has micrometer grade hole at end face, makes the precursor source material alternately get into the reaction cavity system through carrier gas through the pulse performer; And utilize unnecessary precursor source material and the byproduct of reaction of carrier gas cleaning, thereby obtain required micro/nano-scale powder with resist parcel.
10. a kind of micro/nano-scale powder resist packaging method as claimed in claim 9 is characterized in that: the temperature of reaction cavity system is a room temperature to 300 ℃.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103556129A (en) * | 2013-10-31 | 2014-02-05 | 无锡迈纳德微纳技术有限公司 | Method for coating fluorescent powder with nanoscale oxide film by use of atomic layer deposition technology |
| CN105648422A (en) * | 2016-01-14 | 2016-06-08 | 北京大学深圳研究生院 | Gaseous phase atomic layer deposition device for electrode powder material coating and application |
| CN106367732A (en) * | 2016-09-22 | 2017-02-01 | 四川大学 | Device for medium-temperature organometallic chemical vapor deposition of TiO2-Al2O3 composite coating and coating method |
| CN109321895A (en) * | 2017-07-31 | 2019-02-12 | 北京北方华创微电子装备有限公司 | A kind of charge delivery mechanism and its air inlet method for ALD technique |
| CN110273141A (en) * | 2019-08-02 | 2019-09-24 | 华东师范大学 | A kind of chemical vapour deposition reactor furnace for liquid precursor |
| CN111218669A (en) * | 2020-01-10 | 2020-06-02 | 四川大学 | Rotary drum type reactor for pulse chemical vapor deposition coating and application thereof |
| CN112176319A (en) * | 2020-09-01 | 2021-01-05 | 江苏微导纳米科技股份有限公司 | Powder coating device and powder coating method |
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| WO2005112082A1 (en) * | 2004-05-18 | 2005-11-24 | Ips Ltd. | Cyclic pulsed two-level plasma atomic layer deposition apparatus and method |
| CN102127756A (en) * | 2011-02-21 | 2011-07-20 | 东华大学 | Device and method for enhancing atomic layer deposition by pulse-modulation radio frequency plasma |
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Patent Citations (2)
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| WO2005112082A1 (en) * | 2004-05-18 | 2005-11-24 | Ips Ltd. | Cyclic pulsed two-level plasma atomic layer deposition apparatus and method |
| CN102127756A (en) * | 2011-02-21 | 2011-07-20 | 东华大学 | Device and method for enhancing atomic layer deposition by pulse-modulation radio frequency plasma |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103556129A (en) * | 2013-10-31 | 2014-02-05 | 无锡迈纳德微纳技术有限公司 | Method for coating fluorescent powder with nanoscale oxide film by use of atomic layer deposition technology |
| CN103556129B (en) * | 2013-10-31 | 2016-03-02 | 无锡迈纳德微纳技术有限公司 | A kind of technique for atomic layer deposition that utilizes is to the method for fluorescent material clad nano level sull |
| CN105648422A (en) * | 2016-01-14 | 2016-06-08 | 北京大学深圳研究生院 | Gaseous phase atomic layer deposition device for electrode powder material coating and application |
| CN106367732A (en) * | 2016-09-22 | 2017-02-01 | 四川大学 | Device for medium-temperature organometallic chemical vapor deposition of TiO2-Al2O3 composite coating and coating method |
| CN106367732B (en) * | 2016-09-22 | 2018-11-06 | 四川大学 | A kind of medium temperature metal organic chemical vapor deposition TiO2-Al2O3Composite coating device and painting method |
| CN109321895A (en) * | 2017-07-31 | 2019-02-12 | 北京北方华创微电子装备有限公司 | A kind of charge delivery mechanism and its air inlet method for ALD technique |
| CN110273141A (en) * | 2019-08-02 | 2019-09-24 | 华东师范大学 | A kind of chemical vapour deposition reactor furnace for liquid precursor |
| CN111218669A (en) * | 2020-01-10 | 2020-06-02 | 四川大学 | Rotary drum type reactor for pulse chemical vapor deposition coating and application thereof |
| CN111218669B (en) * | 2020-01-10 | 2021-08-17 | 四川大学 | Rotary drum type reactor for pulse chemical vapor deposition coating and application thereof |
| CN112176319A (en) * | 2020-09-01 | 2021-01-05 | 江苏微导纳米科技股份有限公司 | Powder coating device and powder coating method |
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Denomination of invention: Micronano-scale powder protective layer wrapping device and method Effective date of registration: 20140505 Granted publication date: 20130911 Pledgee: Agricultural Bank of China Limited by Share Ltd Wuxi science and Technology Branch Pledgor: Wuxi MNT Micro and Nanotech Co.,Ltd. Registration number: 2014990000324 |
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Effective date of registration: 20171220 Address after: 214100 Jiangsu province Wuxi City Linghu New District Road No. 228 Wu Tian wisdom city 3-104 Patentee after: Jiangsu mynard micro nano technology Co. Ltd. Address before: 214028 room 209, No. 8, Wuxi New District, Wuxi, Jiangsu Patentee before: Wuxi MNT Micro and Nanotech Co.,Ltd. |