CN108754515A - The method for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution - Google Patents
The method for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution Download PDFInfo
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- CN108754515A CN108754515A CN201810469101.1A CN201810469101A CN108754515A CN 108754515 A CN108754515 A CN 108754515A CN 201810469101 A CN201810469101 A CN 201810469101A CN 108754515 A CN108754515 A CN 108754515A
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- ammonium hydroxide
- hydrogen peroxide
- peroxide solution
- titanium
- nitride film
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Mechanical Engineering (AREA)
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- Organic Chemistry (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
A method of titanium and titanium nitride film being removed using ammonium hydroxide hydrogen peroxide solution, including：1, immersion treatment is carried out to workpiece using ammonium hydroxide hydrogen peroxide solution, ammonium hydroxide hydrogen peroxide solution is that volume ratio is H2O2：H2O：NH4OH=3：4：1 is formulated, and soaking temperature is room temperature, and the reaction time is 3-5 hours, until range estimation workpiece surface noresidue titanium film or titanium nitride film position；2, it is rinsed using flowing water, rinsing time is greater than or equal to 30 seconds；3, neutralization reaction is carried out using nitre fluoric acid, nitre fluoric acid is matched using nitric acid and hydrofluoric acid, and the volume ratio of each liquid is HNO3：HF：H2O=20：1：20, it reacts to carry out immersion reaction, reaction time 10-30S at a temperature of room temperature；4, soaking flushing 30 minutes or more is carried out using flowing water, when immersion should keep the flowing of ultra-pure water；5, the workpiece after soaking and washing is placed on the jig of drying oven and is dried.
Description
Technical field
The present invention discloses a kind of overlay film stripping means, especially a kind of to utilize ammonium hydroxide hydrogen peroxide solution stripping titanium and titanium nitride
The method of film.
Background technology
With the continuous development of semiconductor and liquid crystal display panel industry, the semiconductor industry and liquid crystal display panel industry in China
Very big promotion is obtained, industry production capacity is also higher and higher.The industries such as semiconductor and liquid crystal display panel belong to fining industry,
It is very high to production equipment requirement, therefore the parts of equipment is required to need to carry out periodic maintenance, to ensure to produce precision.
The chemical stability of titanium film and titanium nitride film is good, and fusing point is up to 3000 DEG C, and hardness is high, red hardness is good, and has concurrently good
Good toughness, the advantages that wearability is good, therefore, many component surfaces in the process equipments such as semiconductor and liquid crystal display panel
All adhere to one layer of titanium film or titanium nitride film, to keep its performance.However, in such parts maintenance maintenance, need to original
The titanium film or titanium nitride film of attachment are removed, and could carry out the operation of new titanium film or titanium nitride film, and in the prior art, it goes
Usually there is the molten bubble of chemical solution except the titanium film or titanium nitride film of workpiece surface attachment or removed by the way of mechanical stripping, is gone
Except effect is bad, and be easy to damage workpiece itself.
Invention content
Effect is bad when titanium film or titanium nitride film for workpiece surface in the prior art mentioned above remove lacks
Point, the present invention provide a kind of method for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution, utilize ammonium hydroxide and hydrogen peroxide
The titanium or titanium nitride of the method removal workpiece surface attachment chemically reacted, effect are preferable.
The present invention solve its technical problem the technical solution adopted is that：It is a kind of to utilize ammonium hydroxide hydrogen peroxide solution stripping titanium and nitrogen
Change the method for titanium film, this method includes the following steps：
（1）, ammonium hydroxide hydrogen peroxide solution impregnate：Immersion treatment is carried out to workpiece using ammonium hydroxide hydrogen peroxide solution, ammonium hydroxide dioxygen is water-soluble
Liquid is that volume ratio is H2O2：H2O：NH4OH=3：4：1 is formulated, and soaking temperature is room temperature, and the reaction time is 3-5 hours, until
Estimate workpiece surface noresidue titanium film or titanium nitride film position；
（2）, rinsing：It is rinsed using flowing water, rinsing time is greater than or equal to 30 seconds；
（3）, neutralization reaction：Neutralization reaction is carried out using nitre fluoric acid, nitre fluoric acid is matched using nitric acid and hydrofluoric acid, each liquid
Volume ratio be HNO3：HF：H2O=20：1：20, it reacts to carry out immersion reaction, reaction time 10-30S at a temperature of room temperature；
（4）, pure water impregnate：Soaking flushing 30 minutes or more is carried out using flowing water, when immersion should keep the flowing of ultra-pure water；
（5）, it is dry：Workpiece after soaking and washing is placed on the jig of drying oven and is dried.
The technical solution that the present invention solves the use of its technical problem further comprises：
The step（1）The middle ammonium hydroxide hydrogen peroxide solution used is H for volume ratio2O2：H2O：NH4OH=3：4：1.
The step（1）The middle hydrogen peroxide used is the hydrogen peroxide of concentration 30-32%.
The step（1）The ammonium hydroxide that the middle ammonium hydroxide used is 25% for mass percent concentration.
The step（1）When the base material of middle workpiece is Ti, per half an hour, observation is primary.
The step（2）The middle water used is greater than or equal to the ultra-pure water of 12M Ω .CM for resistivity.
The step（3）The volume ratio of each liquid of the middle nitre fluoric acid used is HNO3：HF：H2O =20：1：20.
The step（3）The middle hydrofluoric acid used for a concentration of 55% hydrofluoric acid.
The step（4）The middle water used is greater than or equal to the ultra-pure water of 12M Ω .CM for resistivity.
The step（5）The middle workpiece by after soaking and washing is placed on the jig of drying oven and is dried, and uses
CDA is dried up, and room temperature is blown to surface object circulating water, puts to drying box and be dried, and drying temperature is 150 ± 5 DEG C, is toasted 2 hours
More than.
The beneficial effects of the invention are as follows：The present invention removes workpiece table using the method that ammonium hydroxide and hydrogen peroxide are chemically reacted
The titanium or titanium nitride of face attachment, it is not only efficient, and also removal is clean, thorough, and small to workpiece self-inflicted injury, effect is preferable.
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Description of the drawings
Fig. 1 is operational flowchart of the present invention.
Specific implementation mode
The present embodiment is the preferred embodiment for the present invention, other its all principles and basic structure are identical or close as the present embodiment
As, within the scope of the present invention.
Attached drawing 1 is please referred to, the present invention is mainly a kind of method for removing titanium and titanium nitride film using hydrogen peroxide solution, packet
Include following step：
（1）, workpiece（Or it is component）Confirm, compares the kind of quantity sheet content check workpiece to be processed, include mainly：Workpiece
Base material whether be SUS（That is stainless steel）Or Ti（Titanium）, whether the quantity of workpiece consistent with inventory with specific product, workpiece surface
Whether scuffing, breakage etc. are had；
（2）, ammonium hydroxide hydrogen peroxide solution impregnate：In the present embodiment, immersion treatment, leaching are carried out to workpiece using ammonium hydroxide hydrogen peroxide solution
When bubble, hydrogen peroxide solution of being subject to did not had workpiece, that is, ensured that workpiece is all soaked into hydrogen peroxide solution, in the present embodiment, is adopted
Ammonium hydroxide hydrogen peroxide solution is that volume ratio is H2O2：H2O：NH4OH=（2.5-3.5）：（3.5-4.5）：（0.5-1.5）Prepare and
At, preferably, H2O2：H2O：NH4OH=3：4：1, in the present embodiment, the water used is that resistivity is greater than or equal to 12M Ω .CM
Ultra-pure water, soaking temperature is room temperature, and the reaction time is 3-5 hour, until estimating workpiece surface noresidue titanium film or titanium nitride
Until film, primary every half an hour observation if workpiece base material is Ti, in the present embodiment, hydrogen peroxide is using commercially available
Mass percent concentration be 30 ~ 32% hydrogen peroxide, ammonium hydroxide use commercially available mass percent concentration for 25% ammonium hydroxide；
In the present embodiment, when the hydrogen peroxide concentration in mixed solution is less than 5%, needs to replace soaking solution, replace liquid
It when body, need to be measured using dedicated measurer, need to carry out relevant record work when replacing liquid medicine, pay attention to handling with care,
In order to avoid causing unnecessary loss.
（3）, rinsing：It is rinsed using the ultra-pure water of flowing, rinsing time is greater than or equal to 30 seconds, to clean up work
Part surface, in the present embodiment, the water used is greater than or equal to the ultra-pure water of 12M Ω .CM for resistivity；
（4）, neutralization reaction：Neutralization reaction is carried out using nitre fluoric acid, in the present embodiment, the nitre fluoric acid of use uses nitric acid and hydrogen fluorine
Acid matches, and when proportioning, the volume ratio of each solution is HNO3：HF：H2O=（17~23）：（0.5~1.5）：（17~23）, preferably
HNO3：HF：H2O =20：1：20, in the present embodiment, to react to carry out immersion reaction at a temperature of room temperature, the reaction time is 10 ~
30S, in the present embodiment, the concentrated nitric acid that the nitric acid that uses is 68% for commercially available mass percent concentration, when it is implemented, also may be used
To carry out equivalent proportioning using the nitric acid of other concentration, in the present embodiment, the hydrofluoric acid used is dense for commercially available mass percent
The hydrofluoric acid that degree is 55%, when it is implemented, the nitric acid of other concentration can also be used to carry out equivalent proportioning；
In the present embodiment, when concentration of nitric acid is less than 10%, nitre fluorspar acid solution is needed replacing, when replacing liquid, need to be used dedicated
Measurer is measured, and is needed to carry out relevant record work when replacing liquid medicine, is paid attention to handling with care, in order to avoid cause unnecessary damage
It loses.
（5）, pure water impregnate：Soaking flushing 30 minutes or more is carried out using the ultra-pure water of flowing, when immersion should keep ultrapure
The flowing of water, in the present embodiment, the water used is greater than or equal to the ultra-pure water of 12M Ω .CM for resistivity；
（6）, it is dry：Workpiece after soaking and washing is placed on the jig of drying oven and is dried, (is deoiled using CDA
Water compressed air) it dries up, room temperature is blown to surface object circulating water, puts to drying box and be dried, and drying temperature is 150 ± 5 DEG C, is dried
It is 2 hours or more roasting.
（7）, confirm：Range estimation confirms that whether there is or not residual films, if there is residual film then needs to be handled again, if not residual
Film is stayed then to be confirmed as certified products.
The titanium or titanium nitride for the method removal workpiece surface attachment that the present invention is chemically reacted using ammonium hydroxide and hydrogen peroxide,
It is not only efficient, and removal is clean, thorough, and small to workpiece self-inflicted injury, effect is preferable.
Claims (10)
1. a kind of method for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution, it is characterized in that：Under the method includes
State step：
（1）, ammonium hydroxide hydrogen peroxide solution impregnate：Immersion treatment is carried out to workpiece using ammonium hydroxide hydrogen peroxide solution, ammonium hydroxide dioxygen is water-soluble
Liquid is that volume ratio is H2O2：H2O：NH4OH=（2.5-3.5）：（3.5-4.5）：（0.5-1.5）It is formulated, soaking temperature is normal
Temperature, the reaction time is 3-5 hours, until range estimation workpiece surface noresidue titanium film or titanium nitride film position；
（2）, rinsing：It is rinsed using flowing water, rinsing time is greater than or equal to 30 seconds；
（3）, neutralization reaction：Neutralization reaction is carried out using nitre fluoric acid, nitre fluoric acid is matched using nitric acid and hydrofluoric acid, each liquid
Volume ratio be HNO3：HF：H2O=（17~23）：（0.5~1.5）：（17~23）, react anti-to carry out impregnating at a temperature of room temperature
It answers, reaction time 10-30S；
（4）, pure water impregnate：Soaking flushing 30 minutes or more is carried out using flowing water, when immersion should keep the flowing of ultra-pure water；
（5）, it is dry：Workpiece after soaking and washing is placed on the jig of drying oven and is dried.
2. the method according to claim 1 for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution, it is characterized in that：Institute
The step of stating（1）The middle ammonium hydroxide hydrogen peroxide solution used is H for volume ratio2O2：H2O：NH4OH=3：4：1.
3. the method according to claim 1 for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution, it is characterized in that：Institute
The step of stating（1）The middle hydrogen peroxide used is the hydrogen peroxide of concentration 30-32%.
4. the method according to claim 1 for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution, it is characterized in that：Institute
The step of stating（1）The ammonium hydroxide that the middle ammonium hydroxide used is 25% for mass percent concentration.
5. the method according to claim 1 for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution, it is characterized in that：Institute
The step of stating（1）When the base material of middle workpiece is Ti, per half an hour, observation is primary.
6. the method according to claim 1 for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution, it is characterized in that：Institute
The step of stating（2）The middle water used is greater than or equal to the ultra-pure water of 12M Ω .CM for resistivity.
7. the method according to claim 1 for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution, it is characterized in that：Institute
The step of stating（3）The volume ratio of each liquid of the middle nitre fluoric acid used is HNO3：HF：H2O =20：1：20.
8. the method according to claim 1 for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution, it is characterized in that：Institute
The step of stating（3）The middle hydrofluoric acid used for a concentration of 55% hydrofluoric acid.
9. the method according to claim 1 for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution, it is characterized in that：Institute
The step of stating（4）The middle water used is greater than or equal to the ultra-pure water of 12M Ω .CM for resistivity.
10. the method according to claim 1 for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution, it is characterized in that：
The step（5）The middle workpiece by after soaking and washing is placed on the jig of drying oven and is dried, and is dried up using CDA,
Room temperature is blown to surface object circulating water, puts to drying box and is dried, and drying temperature is 150 ± 5 DEG C, toast 2 hours or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810469101.1A CN108754515A (en) | 2018-05-16 | 2018-05-16 | The method for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution |
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| CN201810469101.1A CN108754515A (en) | 2018-05-16 | 2018-05-16 | The method for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution |
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| CN201810469101.1A Pending CN108754515A (en) | 2018-05-16 | 2018-05-16 | The method for removing titanium and titanium nitride film using ammonium hydroxide hydrogen peroxide solution |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109590267A (en) * | 2018-12-28 | 2019-04-09 | 深圳仕上电子科技有限公司 | Cleaning method |
| CN112176354A (en) * | 2020-09-30 | 2021-01-05 | 久钻科技(成都)有限公司 | Film removing method for physical vapor deposition cutter |
| CN112553630A (en) * | 2020-12-02 | 2021-03-26 | 江苏凯威特斯半导体科技有限公司 | Process for removing titanium or titanium nitride film on surface of semiconductor equipment |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5232619A (en) * | 1990-10-19 | 1993-08-03 | Praxair S.T. Technology, Inc. | Stripping solution for stripping compounds of titanium from base metals |
| CN1209646A (en) * | 1997-08-22 | 1999-03-03 | 日本电气株式会社 | Mfg. method for semiconductor device |
| CN102108482A (en) * | 2009-12-23 | 2011-06-29 | 北大方正集团有限公司 | Method for cleaning spare parts of physical vapor deposition equipment |
| CN105492973A (en) * | 2013-08-28 | 2016-04-13 | 日产化学工业株式会社 | Pattern forming method using resist underlayer film |
| CN105492576A (en) * | 2013-08-30 | 2016-04-13 | 高级技术材料公司 | Compositions and methods for selectively etching titanium nitride |
-
2018
- 2018-05-16 CN CN201810469101.1A patent/CN108754515A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5232619A (en) * | 1990-10-19 | 1993-08-03 | Praxair S.T. Technology, Inc. | Stripping solution for stripping compounds of titanium from base metals |
| CN1209646A (en) * | 1997-08-22 | 1999-03-03 | 日本电气株式会社 | Mfg. method for semiconductor device |
| CN102108482A (en) * | 2009-12-23 | 2011-06-29 | 北大方正集团有限公司 | Method for cleaning spare parts of physical vapor deposition equipment |
| CN105492973A (en) * | 2013-08-28 | 2016-04-13 | 日产化学工业株式会社 | Pattern forming method using resist underlayer film |
| CN105492576A (en) * | 2013-08-30 | 2016-04-13 | 高级技术材料公司 | Compositions and methods for selectively etching titanium nitride |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109590267A (en) * | 2018-12-28 | 2019-04-09 | 深圳仕上电子科技有限公司 | Cleaning method |
| CN112176354A (en) * | 2020-09-30 | 2021-01-05 | 久钻科技(成都)有限公司 | Film removing method for physical vapor deposition cutter |
| CN112553630A (en) * | 2020-12-02 | 2021-03-26 | 江苏凯威特斯半导体科技有限公司 | Process for removing titanium or titanium nitride film on surface of semiconductor equipment |
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Application publication date: 20181106 |