CN105132886B - A kind of method for improving tubular substrate inner surface deposition film uniformity - Google Patents
A kind of method for improving tubular substrate inner surface deposition film uniformity Download PDFInfo
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- CN105132886B CN105132886B CN201510576553.6A CN201510576553A CN105132886B CN 105132886 B CN105132886 B CN 105132886B CN 201510576553 A CN201510576553 A CN 201510576553A CN 105132886 B CN105132886 B CN 105132886B
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- tubular substrate
- air inlet
- inlet pipe
- deposition film
- surface deposition
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Abstract
The invention discloses it is a kind of improve tubular substrate inner surface deposition film uniformity method,（1）Tubular substrate is positioned in reative cell, the air inlet pipe that some through holes are evenly distributed with side wall is placed in the tubular substrate；（2）Tubular substrate is heated；（3）Precursors are passed through into reative cell by the air inlet pipe and carry out plated film.A kind of method for improving tubular substrate inner surface deposition film uniformity of the present invention, the uniformity of tubular substrate inner surface deposition film can be significantly improved.
Description
Technical field
The present invention relates to technique for atomic layer deposition field, especially a kind of improvement tubular substrate inner surface deposition film is uniform
The method of property.
Background technology
Technique for atomic layer deposition is a kind of accurate film deposition techniques, is alternately passed through vaporous precursors instead by pulse
Answer room, and a kind of technology of chemisorbed and reaction film forming in substrate.The surface reaction of ald has from restricted,
I.e. during each pulse, vaporous precursors can only adsorb and react in the atomic bonding position of deposition surface, and reaction reaches saturation
Voluntarily stop afterwards, obtain a monofilm across the deposition surface, therefore, in theory, utilize the thin of technique for atomic layer deposition deposition
Film has good thickness evenness, on a planar base using technique for atomic layer deposition deposition film when, also demonstrate that with pole
High thickness evenness.But when by atomic layer deposition applications in elongated tubular substrate inner surface deposition film, practice card
Bright, film gauge uniformity is poor, shows as that presoma arrival end film is thicker, and the port of export is relatively thin, inhomogeneities up to 30% with
On.
The content of the invention
The present invention in view of the shortcomings of the prior art, proposes a kind of side for improving tubular substrate inner surface deposition film uniformity
Method, the uniformity of tubular substrate inner surface deposition film can be significantly improved.
A kind of method for improving tubular substrate inner surface deposition film uniformity, comprises the following steps：
（1）Tubular substrate is positioned in reative cell, the air inlet pipe that some through holes are evenly distributed with side wall is placed in institute
State in tubular substrate；
（2）Tubular substrate is heated；
（3）Precursors are passed through into reative cell by the air inlet pipe and carry out plated film.
Further, the step（1）Described in air inlet pipe to insert one end of the tubular substrate be blind end.
Further, the blind end is inserted from described tubular substrate one end, stretched out from the other end, and each through hole is located at
Inside the tubular substrate.
Further, the air inlet pipe and the tubular substrate axis coinciding.
Further, the step（2）It is middle that gradient-heated is carried out to it along the tubular substrate length direction, to the pipe
The air inlet pipe insertion of shape substrate heating one end temperature is minimum, other end heating-up temperature highest.
Further, linearly increase to the heating-up temperature of its other end from one end that the air inlet pipe of the tubular substrate is inserted
It is long.
Further, the step（3）Comprise the following steps：
（i）The first precursors is passed through into reative cell;
(ii) argon gas is passed through for the first time；
（iii）Second of precursors is passed through into reative cell
（iv）Argon gas is passed through for the second time
（v）Repeat the above steps（i）Extremely（iv）, untill thicknesses of layers meets to require.
A kind of method for improving tubular substrate inner surface deposition film uniformity of the present invention, by adjusting intake method and anti-
Temperature is answered, the uniformity of film can be significantly improved, technique for atomic layer deposition is efficiently applied to elongated tubular product substrate
Inner surface thin film deposition.
Brief description of the drawings
Fig. 1 is a kind of schematic diagram tubulose of method for improving tubular substrate inner surface deposition film uniformity of the present invention
The structural scheme of mechanism of substrate and air inlet pipe.
Embodiment
The present invention will be described in detail below in conjunction with the accompanying drawings, and the description of this part is only exemplary and explanatory, should not
There is any restriction effect to protection scope of the present invention.
The tubular substrate applied in a kind of method of improvement tubular substrate inner surface deposition film uniformity as shown in Figure 1
1 and the position relationship of air inlet pipe 1,
One end that air inlet pipe 1 stretches into tubular substrate 1 is blind end 21, blind end 21 from the insertion of one end of tubular substrate 1, from
The other end stretches out, air inlet pipe 1 and the axis coinciding of tubular substrate 1.Some through holes 22 are evenly distributed with the side wall of air inlet pipe 1, are surround
Air inlet pipe is evenly distributed with four through holes 22 on 1 same cross section, and four through holes 22 are one group, is axially distributed along air inlet pipe 1
There are some groups, some groups of through holes 22 are located inside tubular substrate 1.
Embodiment 1
The present embodiment is reacted with trimethyl aluminium and vapor, is illustrated exemplified by generation alundum (Al2O3).
(1) tubular substrate 1 for needing plated film is positioned in reative cell, the air inlet pipe 1 that through hole 22 is distributed with is placed in tubulose
Inside substrate 1, air inlet pipe 1 and tubular substrate 1 are axially concentric, and the length of air inlet pipe 1 is slightly longer than the length of tubular substrate 1, outside air inlet pipe 1
Footpath 5mm, wall thickness 0.5mm；At the blind end 2110mm of air inlet pipe 1, one group of four through hole 22, aperture are circumferentially uniformly distributed
1mm, along the axis direction of air inlet pipe 1, it is uniformly distributed multigroup through hole 22, is depended between every group at intervals of 5mm, 22 groups of numbers of through hole
The length of air inlet pipe 1；
(2) reative cell is evacuated to 1 × 10-3Pa；
(3) gradient-heated is carried out to tubular substrate 1, the heating one end temperature that tubular substrate 1 is inserted positioned at air inlet pipe 1 is
200 DEG C, it is 400 DEG C to stretch out the heating one end temperature of tubular substrate 1 positioned at air inlet pipe 1, and thermograde meets linear as far as possible vertically
Relation；
(4) the first precursors trimethyl aluminium (TMA), flow 15sccm, duration are passed through into reative cell
5s, one single adsorption layer is formed with chemisorbed needing the inner surface of tubular substrate 1 of plated film；
(5) argon gas, flow 25sccm, duration 15s, by the first unadsorbed unnecessary are passed through into reative cell
Precursors trimethyl aluminium discharges reative cell；
(6) it is passed through second of precursors vapor (H2O) into reative cell, flow 20sccm, duration 10s,
The first precursors trimethyl aluminium with adsorbing in the inner surface of tubular substrate 1 reacts, the table in the tubular substrate 1 for need plated film
Face generates the monoatomic layer and byproduct methane (CH4) of an aluminum oxide；
(7) argon gas is passed through into reative cell, flow 25sccm, duration 15s are anti-by unreacted unnecessary second
Presoma vapor and byproduct of reaction methane is answered to discharge reative cell；
(8) repeat the above steps (4) to (7), untill thicknesses of layers meets to require.
Embodiment 2
The present embodiment is reacted with stannous chloride and hydrogen, is illustrated exemplified by generation copper.
(1) tubular substrate 1 for needing plated film is positioned in reative cell, the air inlet pipe 1 that passage is distributed with is placed in tubulose
Inside substrate 1, air inlet pipe 1 and tubular substrate 1 are axially concentric, and the length of air inlet pipe 1 is slightly longer than the length of tubular substrate 1, outside air inlet pipe 1
Footpath 8mm, wall thickness 1mm；At the blind end 2110mm of air inlet pipe 1, one group of 4 through hole 22, aperture are circumferentially uniformly distributed
1.5mm, along the axis direction of air inlet pipe 1, it is uniformly distributed multigroup through hole 22, depending at intervals of 8mm, 22 groups of numbers of through hole between every group
In length of tube；
(2) reative cell is evacuated to 2 × 10-3Pa；
(3) gradient-heated is carried out to tubular substrate 1, the heating one end temperature that tubular substrate 1 is inserted positioned at air inlet pipe 1 is
200 DEG C, the heating one end temperature that tubular substrate 1 is stretched out positioned at air inlet pipe 1 is 400 DEG C, and thermograde meets line as far as possible vertically
Sexual intercourse；
(4) the first precursors stannous chloride (CuCl), flow 18sccm, duration are passed through into reative cell
6s, one single adsorption layer is formed with chemisorbed needing the inner surface of tubular substrate 1 of plated film；
(5) argon gas, flow 25sccm, duration 15s, by the first unadsorbed unnecessary are passed through into reative cell
Precursors stannous chloride discharges reative cell；
(6) second of precursors hydrogen (H2), flow 15sccm, duration 8s, with suction are passed through into reative cell
Attached the first precursors stannous chloride reaction, needing the monatomic of the inner surface of tubular substrate 1 one copper of generation of plated film
Layer and byproduct hydrogen chloride (HCl)；
(7) argon gas is passed through into reative cell, flow 25sccm, duration 15s are anti-by unreacted unnecessary second
Presoma hydrogen and byproduct of reaction hydrogen chloride is answered to discharge reative cell；
(8) repeat the above steps (4) to (7), is often repeated once, and a copper monoatomic layer is generated, until thicknesses of layers is expired
Untill foot requires.
Embodiment 3
The present embodiment is reacted with titanium tetrachloride and ammonia, is illustrated exemplified by generation titanium nitride.
(1) tubular substrate 1 for needing plated film is positioned in reative cell, the air inlet pipe 1 that through hole 22 is distributed with is placed in tubulose
Inside substrate 1, air inlet pipe 1 and tubular substrate 1 are axially concentric, and the length of air inlet pipe 1 is slightly longer than the length of tubular substrate 1, outside air inlet pipe 1
Footpath 10mm, wall thickness 1mm；At the blind end 2110mm of air inlet pipe 1, one group of 4 through hole 22, aperture are circumferentially uniformly distributed
1.5mm, along the axis direction of air inlet pipe 1, it is uniformly distributed multigroup through hole 22, being taken at intervals of 10mm, 22 groups of numbers of through hole between every group
Certainly in length of tube；
(2) reative cell is evacuated to 5 × 10-3Pa；
(3) gradient-heated is carried out to tubular substrate 1, the heating-up temperature that the one end of tubular substrate 1 is inserted positioned at air inlet pipe 1 is
300 DEG C, it is 500 DEG C to stretch out the heating one end temperature of tubular substrate 1 positioned at air inlet pipe 1, and thermograde meets linear as far as possible vertically
Relation；
(4) the first precursors titanium tetrachloride (TiCl4), flow 20sccm, duration are passed through into reative cell
5s, one single adsorption layer is formed with chemisorbed needing the inner surface of tubular substrate 1 of plated film；
(5) argon gas, flow 20sccm, duration 10s, by the first unadsorbed unnecessary are passed through into reative cell
Precursors titanium tetrachloride discharges reative cell；
(6) second of precursors ammonia (NH3) is passed through into reative cell, with adsorbing in the inner surface of tubular substrate 1
The first precursors titanium tetrachloride reaction, needing the monatomic of the inner surface of tubular substrate 1 one titanium nitride of generation of plated film
Layer and byproduct hydrogen chloride (HCl)；
(7) it is passed through argon gas into reative cell, flow 25sccm, duration 8s are anti-by unreacted unnecessary second
Presoma ammonia and byproduct of reaction hydrogen chloride is answered to discharge reative cell；
(8) repeat the above steps (4) to (7), untill thicknesses of layers meets to require.
A kind of method for improving tubular substrate inner surface deposition film uniformity of the present invention, by adjusting intake method and anti-
Temperature is answered, the uniformity of film can be significantly improved, technique for atomic layer deposition is efficiently applied to elongated tubular product substrate
Inner surface thin film deposition.
Claims (6)
- A kind of 1. method for improving tubular substrate inner surface deposition film uniformity, it is characterised in that comprise the following steps：（1）Tubular substrate is positioned in reative cell, the air inlet pipe that some through holes are evenly distributed with side wall is placed in the pipe In shape substrate；（2）Gradient-heated is carried out to it along the tubular substrate length direction, one inserted to the air inlet pipe of the tubular substrate End heating-up temperature is minimum, other end heating-up temperature highest；（3）Precursors are passed through into reative cell by the air inlet pipe and carry out plated film；The step（1）In, the distribution mode of through hole is in air inlet pipe：One group of through hole is distributed along air inlet pipe even circumferential, edge is entered Tracheae axis direction, it is uniformly distributed multigroup through hole.
- A kind of 2. method for improving tubular substrate inner surface deposition film uniformity as described in claim 1, it is characterised in that The step（1）Described in air inlet pipe to insert one end of the tubular substrate be blind end.
- A kind of 3. method for improving tubular substrate inner surface deposition film uniformity as described in claim 2, it is characterised in that The blind end is inserted from described tubular substrate one end, stretched out from the other end, and each through hole is located inside the tubular substrate.
- 4. a kind of method for improving tubular substrate inner surface deposition film uniformity as described in claim 1 to 3 is any, it is special Sign is, the air inlet pipe and the tubular substrate axis coinciding.
- A kind of 5. method for improving tubular substrate inner surface deposition film uniformity as claimed in claim 1, it is characterised in that institute State step（2）In, linearly increase to the heating-up temperature of its other end from one end that the air inlet pipe of the tubular substrate is inserted.
- A kind of 6. method for improving tubular substrate inner surface deposition film uniformity as described in claim 1, it is characterised in that The step（3）Comprise the following steps：（i）The first precursors is passed through into reative cell;(ii) argon gas is passed through for the first time；（iii）Second of precursors is passed through into reative cell（iv）Argon gas is passed through for the second time（v）Repeat the above steps（i）Extremely（iv）, untill thicknesses of layers meets to require.
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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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|---|---|---|---|
| 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 CN105132886A (en) | 2015-12-09 |
| CN105132886B true CN105132886B (en) | 2018-03-23 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108559977B (en) * | 2018-01-22 | 2020-11-20 | 大连理工大学 | Method and equipment for low-temperature coating on inner wall of slender metal pipe |
| 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 |
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 |
-
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 |
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