CN106435589A - Chromium etching liquid and preparation method thereof - Google Patents
Chromium etching liquid and preparation method thereof Download PDFInfo
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- CN106435589A CN106435589A CN201610806796.9A CN201610806796A CN106435589A CN 106435589 A CN106435589 A CN 106435589A CN 201610806796 A CN201610806796 A CN 201610806796A CN 106435589 A CN106435589 A CN 106435589A
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/26—Acidic compositions for etching refractory metals
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- Organic Chemistry (AREA)
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- ing And Chemical Polishing (AREA)
Abstract
The invention discloses chromium etching liquid and a preparation method thereof. The chromium etching liquid comprises 30 to 60 parts of ammonium cerium nitrate, 200 to 300 parts of perchloric acid and 4500 to 6000 parts of deionized water; the preparation method of the chromium etching liquid comprises the following steps: pouring the 30 to 60 parts of ammonium cerium nitrate, the 200 to 300 parts of perchloric acid and the 4500 to 6000 parts of deionized water into a stirring kettle; stirring and mixing at different stirring speeds; vacuumizing after the components are uniformly mixed; and conditioning for a certain time and carrying out filtering. The chromium etching liquid disclosed by the invention can be applied to a bidirectional etching process in which vertical etching and lateral etching can be simultaneously implemented, can be used for realizing precise control of the etching process, and can improve the pattern precision and the precision uniformity of a chromium membrane.
Description
Technical field
The present invention relates to a kind of chromium etching solution and preparation method thereof, belong to the technology neck of chromium etching solution in chromium film etch process
Domain.
Background technology
Chromium film etching process is important technical links, the pattern precision to chromium film mask plate and the essence that chromium film mask plate manufactures
The impact of degree uniformity is very high.Meanwhile, etching solution is an important link in etching process, and wherein ammonium ceric nitrate composition is chromium
One of composition that etching solution is commonly used, there is chemical reaction with the layers of chrome on chromium plate in it, and so that chromium is dissolved in etching solution.As
CN102505118B, provides a kind of environment of aqueous solution of nitric acid, makes ammonium ceric nitrate, with chromium film, chemical reaction occur, and by carrying
The consumption of high nitric acid is improving etching speed；CN102277573B adopts o-fluorobenzoic acid to provide sour environment, still can lead to
Cross consumption to adjust etching speed.
LTPS low-temperature polysilicon silicon technology has become as a relatively complete technology of development, has been widely used in luminous
In panel, its advantage is that luminescent panel has bigger visible angle (being such as applied to bent screen smart mobile phone), and color rendition is good, draws
Face is more life-like gorgeous.In the 5.5th generation that this technology is released successively, the 6th generation production line requires more next to the pattern precision of mask plate
Higher.Due to the two-way etching of this technical requirements chromium film, it is etched from the vertical direction of chromium film to be etched and both sides simultaneously.
Aforesaid existing etching solution etching speed is big, is unfavorable for the precise controlling of etching process, and the etching solution using prior art
When being operated, the speed of vertical etching be more than lateral, because two-way etching can not complete simultaneously, to mask plate patterns precision with
And uniform precision impact is greatly, cause end product fraction defective high.
Content of the invention
The present invention provides a kind of chromium etching solution and preparation method thereof, this etching solution can be applicable to carry out simultaneously vertical etching and
The two-way etch process of chromium film of lateral etch, effectively reduces vertical etch rate, thus reaching equilibrium with lateral etch rate, carries
High chromium film pattern precision and uniform precision.
The present invention is to be realized by following technical scheme：
A kind of chromium etching solution, including following component and content：
30～60 parts of ammonium ceric nitrate；
200～300 parts of perchloric acid；
4500～6000 parts of deionized water.
The present inventor, when being etched liquid research, finds when preparing etching solution using high chloro acid solution,
The effect slowing down etching can be played, make product sideline more smooth simultaneously.In experimentation, first by formula be nitre
600～800 parts of sour cerium ammonium, 200～400 parts of perchloric acid, 4000～5000 parts of deionized water, vertical etch rate now is 14
Angstroms per second～20 angstroms per second, on the chromium film to be etched that experiment is chosen, the response time needs 50～80 seconds although effectively reducing
The etching speed of prior art, but time of completing of the lateral etch simultaneously carrying out be about 1/2nd of vertical etching, still
So need to adjust formula further.
In the experiment subsequently carrying out, inventor is found that the pass that ammonium ceric nitrate concentration change affects on vertical etch rate
System, as shown in Fig. 2 in the aqueous solution of perchloric acid, can make etching speed using low concentration or the ammonium ceric nitrate of high concentration
Decline, but low concentration ammonium ceric nitrate be simultaneously again to can improve pattern precision, therefore select the chromium etching solution of formula of the present invention.
Present invention also offers the preparation method of this etching solution：Realized by below step：
(3) by 30～60 parts of ammonium ceric nitrate, 200～300 parts of perchloric acid and 4500～6000 parts of deionized water pour stirring into
In kettle, stirring simultaneously mix homogeneously, stop evacuation after stirring；
(4) etching solution of above-mentioned mix homogeneously is filtered.
Mixing speed in described step (1) is specially：It is stirred 15 minutes with 500RPM, then stirred with 800RPM
Mix 20 minutes, be finally stirred 15 minutes with 300RPM.
It is evacuated to 0.01～0.08Mpa in described step (1).
Filtration in described step (2) uses FPTE filter, and filter opening is 0.1 μm.
The present invention is applied in vertical and lateral two-way chromium etch process.
Beneficial effects of the present invention are：
1. effectively reduce vertical etch rate, vertical etch rate can be reduced to 7 angstroms per second～9 angstroms per second, from
And make vertical etching time lengthening to 120～150 seconds.
2. etching precision and etch uniformity control are substantially elevated, and end product effect is good.
3. because ammonium ceric nitrate is rare earth compound, present invention reduces raw material use cost, solution is gentle, simplifies
Conservation environment.
Brief description
Fig. 1 is the schematic diagram of two-way etch process
1- vertical etching；2- lateral etch；3- base plate glass；4- chromium film；5- photoresist layer；6- chromium to be etched film.
Fig. 2 is the curve chart that ammonium ceric nitrate concentration change affects vertical etch rate
Wherein etching period unit is the second, and ammonium ceric nitrate usage amount is milliliter number.
Specific embodiment
With reference to embodiments, the present invention will be further described.
Embodiment 1
By 30 parts of ammonium ceric nitrate, 200 parts of perchloric acid and 4500 parts of deionized water are poured in stirred tank and are mixed, and setting is stirred
Mix speed, be first stirred 15 minutes with 500RPM, then be stirred 20 minutes with 800RPM, be finally stirred with 300RPM
15 minutes.Evacuation after stopping, vacuum is maintained at 0.01Mpa, evacuation 15 minutes, and standing, is 0.1 μm with filter opening
FPTE filter is filtered, and puts in HDPE bucket after the completion of filtration.
Embodiment 2
By 60 parts of ammonium ceric nitrate, 300 parts of perchloric acid and 6000 parts of deionized water are poured in stirred tank and are mixed, and setting is stirred
Mix speed, be first stirred 15 minutes with 500RPM, then be stirred 20 minutes with 800RPM, be finally stirred with 300RPM
15 minutes.Evacuation after stopping, vacuum is maintained at 0.08Mpa, evacuation 15 minutes, and standing, is 0.1 μm with filter opening
FPTE filter is filtered, and puts in HDPE bucket after the completion of filtration.
Embodiment 3
By 45 parts of ammonium ceric nitrate, 250 parts of perchloric acid and 5250 parts of deionized water are poured in stirred tank and are mixed, and setting is stirred
Mix speed, be first stirred 15 minutes with 500RPM, then be stirred 20 minutes with 800RPM, be finally stirred with 300RPM
15 minutes.Evacuation after stopping, vacuum is maintained at 0.04Mpa, evacuation 15 minutes, and standing, is 0.1 μm with filter opening
FPTE filter is filtered, and puts in HDPE bucket after the completion of filtration.
Embodiment 4
By 30 parts of ammonium ceric nitrate, 300 parts of perchloric acid and 6000 parts of deionized water are poured in stirred tank and are mixed, and setting is stirred
Mix speed, be first stirred 15 minutes with 500RPM, then be stirred 20 minutes with 800RPM, be finally stirred with 300RPM
15 minutes.Evacuation after stopping, vacuum is maintained at 0.04Mpa, evacuation 15 minutes, and standing, is 0.1 μm with filter opening
FPTE filter is filtered, and puts in HDPE bucket after the completion of filtration.
Embodiment 5
By 60 parts of ammonium ceric nitrate, 200 parts of perchloric acid and 5000 parts of deionized water are poured in stirred tank and are mixed, and setting is stirred
Mix speed, be first stirred 15 minutes with 500RPM, then be stirred 20 minutes with 800RPM, be finally stirred with 300RPM
15 minutes.Evacuation after stopping, vacuum is maintained at 0.06Mpa, evacuation 15 minutes, and standing, is 0.1 μm with filter opening
FPTE filter is filtered, and puts in HDPE bucket after the completion of filtration.
Comparative example
Choosing formula during inventor initially tests is 600～800 parts of ammonium ceric nitrate, 200～400 parts of perchloric acid, deionization
Five group of formula of the chromium etching solution of 4000～5000 parts of water carry out contrasting reference.
Embodiment 1-5 and a few group of formula of comparative example are carried out photoetching CD uniformity test.
Choose identical chromium to be etched film and carry out vertical and lateral etch simultaneously, test photoetching CD uniformity.As table 1.
Table 1
| CD uniformity | Maximum | Minima | Meansigma methodss | Value journey |
| Embodiment 1-5 | 10.1072 | 10.0299 | 10.06308 | 0.0773 |
| 5 groups of comparative example | 10.2747 | 10.0272 | 10.1079 | 0.2475 |
As can be known from Table 1, the value journey of chromium etching solution of the present invention is significantly smaller, that is, have chosen optimal ratio in formula, cover
Film version precision and uniformity controlling are good.
Claims (7)
1. a kind of chromium etching solution is it is characterised in that include following component and content：
30～60 parts of ammonium ceric nitrate；
200～300 parts of perchloric acid；
4500～6000 parts of deionized water.
2. a kind of preparation method of etching solution：Realized by below step：
(1) by 30～60 parts of ammonium ceric nitrate, 200～300 parts of perchloric acid and 4500～6000 parts of deionized water are poured in stirred tank,
Stirring mix homogeneously, stop evacuation after stirring；
(2) etching solution of above-mentioned mix homogeneously is filtered.
3. as claimed in claim 2 a kind of preparation method of etching solution it is characterised in that mixing speed in described step (1)
It is specially：It is stirred 15 minutes with 500RPM, then is stirred 20 minutes with 800RPM, be finally stirred 15 with 300RPM
Minute.
4. as claimed in claim 2 a kind of preparation method of etching solution it is characterised in that being evacuated in described step (1)
0.01～0.08Mpa.
5. as claimed in claim 2 a kind of preparation method of etching solution it is characterised in that filtration in described step (2) uses
FPTE filter, filter opening is 0.1 μm.
6. a kind of chromium etching solution as claimed in claim 1 is it is characterised in that etching speed can be reduced.
7. a kind of chromium etching solution as claimed in claim 1 is it is characterised in that be applied to vertical and lateral two-way chromium etching work
In skill.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610806796.9A CN106435589A (en) | 2016-09-07 | 2016-09-07 | Chromium etching liquid and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610806796.9A CN106435589A (en) | 2016-09-07 | 2016-09-07 | Chromium etching liquid and preparation method thereof |
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| CN106435589A true CN106435589A (en) | 2017-02-22 |
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| CN201610806796.9A Pending CN106435589A (en) | 2016-09-07 | 2016-09-07 | Chromium etching liquid and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112048719A (en) * | 2020-08-27 | 2020-12-08 | 江苏中德电子材料科技有限公司 | Chromium metal etching solution and method for etching chromium film and chromium-nickel film |
| CN112087878A (en) * | 2020-09-14 | 2020-12-15 | 深圳市志凌伟业光电有限公司 | Etching method of composite copper film structure |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050075275A (en) * | 2004-01-15 | 2005-07-20 | 동우 화인켐 주식회사 | Integrated etchant composition for chromium (or chromium alloy) single layer and multi layers |
| CN102505118A (en) * | 2011-09-20 | 2012-06-20 | 绵阳艾萨斯电子材料有限公司 | OLED (organic light emitting diode) chromium etchant, preparation method for same and application thereof |
-
2016
- 2016-09-07 CN CN201610806796.9A patent/CN106435589A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050075275A (en) * | 2004-01-15 | 2005-07-20 | 동우 화인켐 주식회사 | Integrated etchant composition for chromium (or chromium alloy) single layer and multi layers |
| CN102505118A (en) * | 2011-09-20 | 2012-06-20 | 绵阳艾萨斯电子材料有限公司 | OLED (organic light emitting diode) chromium etchant, preparation method for same and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112048719A (en) * | 2020-08-27 | 2020-12-08 | 江苏中德电子材料科技有限公司 | Chromium metal etching solution and method for etching chromium film and chromium-nickel film |
| CN112087878A (en) * | 2020-09-14 | 2020-12-15 | 深圳市志凌伟业光电有限公司 | Etching method of composite copper film structure |
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