CN105132886A - Method for improving uniformity of film deposited on inner surface of tubular base - Google Patents
Method for improving uniformity of film deposited on inner surface of tubular base Download PDFInfo
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- CN105132886A CN105132886A CN201510576553.6A CN201510576553A CN105132886A CN 105132886 A CN105132886 A CN 105132886A CN 201510576553 A CN201510576553 A CN 201510576553A CN 105132886 A CN105132886 A CN 105132886A
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- tubular substrate
- inlet pipe
- internal surface
- reaction chamber
- surface deposit
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Abstract
The invention discloses a method for improving the uniformity of a film deposited on the inner surface of a tubular base. The method comprises the following steps: (1) placing the tubular base in a reaction chamber, and placing an air inlet pipe in the tubular base, wherein a plurality of through holes are evenly distributed in the lateral wall of the air inlet pipe; (2) heating the tubular base; and (3) enabling a reaction precursor to be inlet into the reaction chamber through the air inlet pipe so as to perform film coating. By the method for improving the uniformity of the film deposited on the inner surface of the tubular base, disclosed by the invention, the uniformity of the film deposited on the inner surface of the tubular base can be observably improved.
Description
Technical field
The present invention relates to technique for atomic layer deposition field, especially a kind of method improving tubular substrate internal surface deposit film homogeneity.
Background technology
Technique for atomic layer deposition is a kind of film deposition techniques of precision, alternately vaporous precursors is passed into reaction chamber by pulse, and in substrate chemisorption and reaction film forming a kind of technology.The surface reaction of ald has from restricted, namely at each impulse duration, vaporous precursors can only adsorb in the atomic bonding position of deposition surface and react, namely stop voluntarily after reaction reaches capacity, obtain a unitary film across the deposition surface, therefore, in theory, the film utilizing technique for atomic layer deposition to deposit has good thickness evenness, when utilizing technique for atomic layer deposition deposit film on a planar base, also proves to have high thickness evenness.But, by atomic layer deposition applications when elongated tubular substrate internal surface deposit film, facts have proved, film gauge uniformity is poor, and show as presoma inlet end film thicker, exit end is thinner, and ununiformity can reach more than 30%.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, propose a kind of method improving tubular substrate internal surface deposit film homogeneity, significantly can improve the homogeneity of tubular substrate internal surface deposit film.
Improve a method for tubular substrate internal surface deposit film homogeneity, comprise the following steps:
(1) tubular substrate is positioned in reaction chamber, inlet pipe sidewall being evenly distributed with some through holes is placed in described tubular substrate;
(2) tubular substrate is heated;
(3) in reaction chamber, pass into precursors by described inlet pipe and carry out plated film.
Further, the inlet pipe described in described step (1) inserts one end of described tubular substrate is blind end.
Further, described blind end inserts from described tubular substrate one end, stretches out from the other end, and it is inner that each described through hole is positioned at described tubular substrate.
Further, described inlet pipe and described tubular substrate axis coinciding.
Further, carry out gradient-heated in described step (2) along described tubular substrate length direction to it, the heating one end temperature inserted the inlet pipe of described tubular substrate is minimum, the other end Heating temperature is the highest.
Further, linearly increase from one end that the inlet pipe of described tubular substrate is inserted to the Heating temperature of its other end.
Further, described step (3) comprises the following steps:
(i) in reaction chamber, pass into the first precursors;
(ii) first time passes into argon gas;
(iii) in reaction chamber, pass into the second precursors
(iv) second time passes into argon gas
(v) repeat above-mentioned steps (i) to (iv), until thicknesses of layers meets the demands.
A kind of method improving tubular substrate internal surface deposit film homogeneity of the present invention, by regulating intake method and temperature of reaction, significantly can improve the homogeneity of film, make technique for atomic layer deposition effectively can be applied to the internal surface thin film deposition of elongated tubular product substrate.
Accompanying drawing explanation
Fig. 1 is a kind of schematic diagram tubular substrate of method and structural scheme of mechanism of inlet pipe improving tubular substrate internal surface deposit film homogeneity of the present invention.
Embodiment
Describe the present invention below in conjunction with accompanying drawing, the description of this part is only exemplary and explanatory, should not have any restriction to protection scope of the present invention.
A kind of position relationship improving the tubular substrate 1 and inlet pipe 1 applied in the method for tubular substrate internal surface deposit film homogeneity as shown in Figure 1,
One end that inlet pipe 1 stretches into tubular substrate 1 is blind end 21, and blind end 21 inserts from one end of tubular substrate 1, stretches out from the other end, inlet pipe 1 and tubular substrate 1 axis coinciding.Inlet pipe 1 sidewall is evenly distributed with some through holes 22, is evenly distributed with four through holes 22 around on the same cross section of inlet pipe 1, these four through holes 22 are one group, have some groups along inlet pipe 1 axial distribution, and it is inner that these some groups of through holes 22 are positioned at tubular substrate 1.
Embodiment 1
The present embodiment is with trimethyl aluminium and water vapour reaction, and generating aluminium sesquioxide is example explanation.
(1) will the tubular substrate 1 of plated film be needed to be positioned in reaction chamber, the inlet pipe 1 being distributed with through hole 22 is placed in tubular substrate 1 inner, inlet pipe 1 is axially concentric with tubular substrate 1, and inlet pipe 1 length is slightly longer than tubular substrate 1 length, inlet pipe 1 external diameter 5mm, wall thickness 0.5mm; At distance inlet pipe 1 blind end 2110mm place, be circumferentially uniformly distributed one group of four through hole 22, aperture 1mm, along inlet pipe 1 axis direction, be uniformly distributed and organize through hole 22 more, be spaced apart 5mm often between group, through hole 22 groups of numbers depend on inlet pipe 1 length;
(2) reaction chamber is evacuated to 1 × 10
-3pa;
(3) carry out gradient-heated to tubular substrate 1, the heating one end temperature being positioned at inlet pipe 1 tubular substrate 1 is 200 DEG C, and being positioned at inlet pipe 1, to stretch out tubular substrate 1 heating one end temperature be 400 DEG C, and thermograde meets linear relationship vertically as far as possible;
(4) in reaction chamber, passing into the first precursors trimethyl aluminium (TMA), flow 15sccm, time length 5s, forming a single adsorption layer needing tubular substrate 1 internal surface of plated film with chemisorption;
(5) in reaction chamber, pass into argon gas, flow 25sccm, time length 15s, the first the unnecessary precursors trimethyl aluminium do not adsorbed is discharged reaction chamber;
(6) in reaction chamber, the second precursors water vapour (H2O) is passed into, flow 20sccm, time length 10s, react with the first the precursors trimethyl aluminium being adsorbed on tubular substrate 1 internal surface, the monoatomic layer and the byproduct methane (CH4) that are needing tubular substrate 1 internal surface of plated film to generate an aluminum oxide;
(7) in reaction chamber, pass into argon gas, flow 25sccm, time length 15s, unreacted unnecessary the second precursors water vapour and byproduct of reaction methane are discharged reaction chamber;
(8) above-mentioned steps (4) is repeated to (7), until thicknesses of layers meets the demands.
Embodiment 2
The present embodiment is with cuprous chloride and hydrogen reaction, and generating copper is example explanation.
(1) will the tubular substrate 1 of plated film be needed to be positioned in reaction chamber, the inlet pipe 1 being distributed with ventilating pit is placed in tubular substrate 1 inner, inlet pipe 1 is axially concentric with tubular substrate 1, and inlet pipe 1 length is slightly longer than tubular substrate 1 length, inlet pipe 1 external diameter 8mm, wall thickness 1mm; At distance inlet pipe 1 blind end 2110mm place, be circumferentially uniformly distributed one group of 4 through hole 22, aperture 1.5mm, along inlet pipe 1 axis direction, be uniformly distributed and organize through hole 22 more, be spaced apart 8mm often between group, through hole 22 groups of numbers depend on length of tube;
(2) reaction chamber is evacuated to 2 × 10
-3pa;
(3) carry out gradient-heated to tubular substrate 1, the heating one end temperature being positioned at inlet pipe 1 tubular substrate 1 is 200 DEG C, and being positioned at the heating one end temperature that inlet pipe 1 stretches out tubular substrate 1 is 400 DEG C, and thermograde meets linear relationship vertically as far as possible;
(4) in reaction chamber, passing into the first precursors cuprous chloride (CuCl), flow 18sccm, time length 6s, forming a single adsorption layer needing tubular substrate 1 internal surface of plated film with chemisorption;
(5) in reaction chamber, pass into argon gas, flow 25sccm, time length 15s, the first the unnecessary precursors cuprous chloride do not adsorbed is discharged reaction chamber;
(6) in reaction chamber, the second precursors hydrogen (H2) is passed into, flow 15sccm, time length 8s, react with the first precursors cuprous chloride of absorption, the monoatomic layer and the byproduct hydrogen chloride (HCl) that are needing tubular substrate 1 internal surface of plated film to generate a copper;
(7) in reaction chamber, pass into argon gas, flow 25sccm, time length 15s, unreacted unnecessary the second precursors hydrogen and byproduct of reaction hydrogenchloride are discharged reaction chamber;
(8) repeat above-mentioned steps (4) to (7), often repeat once, generate a copper monoatomic layer, until thicknesses of layers meets the demands.
Embodiment 3
The present embodiment is with titanium tetrachloride and ammonia gas react, and generating titanium nitride is example explanation.
(1) will the tubular substrate 1 of plated film be needed to be positioned in reaction chamber, the inlet pipe 1 being distributed with through hole 22 is placed in tubular substrate 1 inner, inlet pipe 1 is axially concentric with tubular substrate 1, and inlet pipe 1 length is slightly longer than tubular substrate 1 length, inlet pipe 1 external diameter 10mm, wall thickness 1mm; At distance inlet pipe 1 blind end 2110mm place, be circumferentially uniformly distributed one group of 4 through hole 22, aperture 1.5mm, along inlet pipe 1 axis direction, be uniformly distributed and organize through hole 22 more, be spaced apart 10mm often between group, through hole 22 groups of numbers depend on length of tube;
(2) reaction chamber is evacuated to 5 × 10
-3pa;
(3) carry out gradient-heated to tubular substrate 1, the Heating temperature being positioned at inlet pipe 1 tubular substrate 1 one end is 300 DEG C, and being positioned at inlet pipe 1, to stretch out tubular substrate 1 heating one end temperature be 500 DEG C, and thermograde meets linear relationship vertically as far as possible;
(4) in reaction chamber, passing into the first precursors titanium tetrachloride (TiCl4), flow 20sccm, time length 5s, forming a single adsorption layer needing tubular substrate 1 internal surface of plated film with chemisorption;
(5) in reaction chamber, pass into argon gas, flow 20sccm, time length 10s, the first the unnecessary precursors titanium tetrachloride do not adsorbed is discharged reaction chamber;
(6) in reaction chamber, the second precursors ammonia (NH3) is passed into, with the first the precursors titanium tetrachloride reaction being adsorbed on tubular substrate 1 internal surface, the monoatomic layer and the byproduct hydrogen chloride (HCl) that are needing tubular substrate 1 internal surface of plated film to generate a titanium nitride;
(7) in reaction chamber, pass into argon gas, flow 25sccm, time length 8s, unreacted unnecessary the second precursors ammonia and byproduct of reaction hydrogenchloride are discharged reaction chamber;
(8) above-mentioned steps (4) is repeated to (7), until thicknesses of layers meets the demands.
A kind of method improving tubular substrate internal surface deposit film homogeneity of the present invention, by regulating intake method and temperature of reaction, significantly can improve the homogeneity of film, make technique for atomic layer deposition effectively can be applied to the internal surface thin film deposition of elongated tubular product substrate.
Claims (7)
1. improve a method for tubular substrate internal surface deposit film homogeneity, it is characterized in that, comprise the following steps:
(1) tubular substrate is positioned in reaction chamber, inlet pipe sidewall being evenly distributed with some through holes is placed in described tubular substrate;
(2) tubular substrate is heated;
(3) in reaction chamber, pass into precursors by described inlet pipe and carry out plated film.
2. a kind of method improving tubular substrate internal surface deposit film homogeneity as claimed in claim 1, it is characterized in that, one end that the inlet pipe described in described step (1) inserts described tubular substrate is blind end.
3. a kind of method improving tubular substrate internal surface deposit film homogeneity as claimed in claim 2, it is characterized in that, described blind end inserts from described tubular substrate one end, stretches out from the other end, and it is inner that each described through hole is positioned at described tubular substrate.
4. a kind of method improving tubular substrate internal surface deposit film homogeneity as described in as arbitrary in claims 1 to 3, is characterized in that, described inlet pipe and described tubular substrate axis coinciding.
5. a kind of method improving tubular substrate internal surface deposit film homogeneity as claimed in claim 1, it is characterized in that, carry out gradient-heated along described tubular substrate length direction to it in described step (2), the heating one end temperature inserted the inlet pipe of described tubular substrate is minimum, the other end Heating temperature is the highest.
6. a kind of method improving tubular substrate internal surface deposit film homogeneity as claimed in claim 5, is characterized in that, linearly increase from one end that the inlet pipe of described tubular substrate is inserted to the Heating temperature of its other end.
7. a kind of method improving tubular substrate internal surface deposit film homogeneity as claimed in claim 1, it is characterized in that, described step (3) comprises the following steps:
(i) in reaction chamber, pass into the first precursors;
(ii) first time passes into argon gas;
(iii) in reaction chamber, pass into the second precursors
(iv) second time passes into argon gas
(v) repeat above-mentioned steps (i) to (iv), until thicknesses of layers meets the demands.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510576553.6A CN105132886B (en) | 2015-09-11 | 2015-09-11 | A kind of method for improving tubular substrate inner surface deposition film uniformity |
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|---|---|---|---|
| CN201510576553.6A CN105132886B (en) | 2015-09-11 | 2015-09-11 | A kind of method for improving tubular substrate inner surface deposition film uniformity |
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| CN105132886A true CN105132886A (en) | 2015-12-09 |
| CN105132886B CN105132886B (en) | 2018-03-23 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559977A (en) * | 2018-01-22 | 2018-09-21 | 大连理工大学 | A kind of method and apparatus in slender metal pipe inner wall low temperature coating |
| CN109295414A (en) * | 2018-12-11 | 2019-02-01 | 北京师范大学 | The technology and equipment of plated film in a kind of deep hole |
| CN112746265A (en) * | 2020-12-29 | 2021-05-04 | 兰州空间技术物理研究所 | Method for preparing coating on inner surface of spray pipe |
Citations (4)
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|---|---|---|---|---|
| US6042652A (en) * | 1999-05-01 | 2000-03-28 | P.K. Ltd | Atomic layer deposition apparatus for depositing atomic layer on multiple substrates |
| CN1795290A (en) * | 2003-05-27 | 2006-06-28 | 应用材料股份有限公司 | Method and apparatus for generating a precursor for a semiconductor processing system |
| CN102598286A (en) * | 2009-09-06 | 2012-07-18 | 张晗钟 | Tubular photovoltaic device and method of making |
| CN103451624A (en) * | 2012-05-30 | 2013-12-18 | 北大方正集团有限公司 | Deposition furnace tube and method for depositing thin films |
-
2015
- 2015-09-11 CN CN201510576553.6A patent/CN105132886B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6042652A (en) * | 1999-05-01 | 2000-03-28 | P.K. Ltd | Atomic layer deposition apparatus for depositing atomic layer on multiple substrates |
| CN1795290A (en) * | 2003-05-27 | 2006-06-28 | 应用材料股份有限公司 | Method and apparatus for generating a precursor for a semiconductor processing system |
| CN102598286A (en) * | 2009-09-06 | 2012-07-18 | 张晗钟 | Tubular photovoltaic device and method of making |
| CN103451624A (en) * | 2012-05-30 | 2013-12-18 | 北大方正集团有限公司 | Deposition furnace tube and method for depositing thin films |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559977A (en) * | 2018-01-22 | 2018-09-21 | 大连理工大学 | A kind of method and apparatus in slender metal pipe inner wall low temperature coating |
| CN109295414A (en) * | 2018-12-11 | 2019-02-01 | 北京师范大学 | The technology and equipment of plated film in a kind of deep hole |
| CN109295414B (en) * | 2018-12-11 | 2020-11-20 | 北京师范大学 | Technology and equipment for coating film in deep hole |
| CN112746265A (en) * | 2020-12-29 | 2021-05-04 | 兰州空间技术物理研究所 | Method for preparing coating on inner surface of spray pipe |
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| CN105132886B (en) | 2018-03-23 |
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