CN106884167A - A kind of hydrogen peroxide stabilizer and hydrogen peroxide etching solution - Google Patents
A kind of hydrogen peroxide stabilizer and hydrogen peroxide etching solution Download PDFInfo
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- CN106884167A CN106884167A CN201510937359.6A CN201510937359A CN106884167A CN 106884167 A CN106884167 A CN 106884167A CN 201510937359 A CN201510937359 A CN 201510937359A CN 106884167 A CN106884167 A CN 106884167A
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- hydrogen peroxide
- etching solution
- stabilizer
- etching
- peroxide stabilizer
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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
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Abstract
The invention discloses a kind of hydrogen peroxide stabilizer and hydrogen peroxide etching solution, belong to metal etch field.Number in the hydrogen peroxide stabilizer simultaneously containing carbon atom in alcoholic extract hydroxyl group and ehter bond, and the hydrogen peroxide stabilizer is 3-12.The present invention provide with constituted above hydrogen peroxide stabilizer, when using it in the metal etch liquid of hydrogen peroxide system, its decomposition that can substantially suppress hydrogen peroxide, and be etched using the etching solution containing the hydrogen peroxide stabilizer, metal material surface after etching will not kish, beneficial to the homogeneity for improving etching.It can be seen that, hydrogen peroxide stabilizer provided in an embodiment of the present invention can not only be improved stability in use and the shelf-life of hydrogen peroxide system etching solution, and beneficial to the etch effect of guarantee hydrogen peroxide system etching solution.
Description
Technical field
The present invention relates to metal etch field, more particularly to a kind of hydrogen peroxide stabilizer and hydrogen peroxide etching solution.
Background technology
Wet-type etching is the conventional means that semicon industry obtains thin type precision microelectronic product, and it is generally comprised
Following three step：(1) metal etch liquid is made to diffuse to metal material surface to be etched；(2) metal is made
Etching solution chemically reacts with metal material to be etched；(3) metal of the reacted product from after etching
Material surface is diffused in solution, and is discharged with solution.The metal etch liquid of hydrogen peroxide system is used as conventional
Etching solution system, it is constant and easy to control with etch-rate, hold the advantages of amount of metal is big, and post processing is simple,
It is widely used in Wet-type etching field.However, in the metal etch liquid of hydrogen peroxide system, due to often needing
Addition inorganic salts carry out the pH of regulation system, so as to the directive property for meeting each metalloid is etched, while reaching specific
Etch-rate, but the metal ion and the change of system pH that are introduced in inorganic salts can reduce hydrogen peroxide
Stability, and then reduce the etching performance of metal etch liquid.It can be seen that, it is necessary in the metal of hydrogen peroxide system
Hydrogen peroxide stabilizer is introduced in etching solution to improve the stability of hydrogen peroxide.
Prior art generally in the metal etch liquid of hydrogen peroxide system add waterglass, ethylenediamine tetra-acetic acid and
Its salt, phosphonic acids and phosphonate as hydrogen peroxide stabilizer, they can by absorption, complexing or chelation,
Combined with the metal ion introduced in inorganic salts in system, it decomposed to block metal ion catalysis hydrogen peroxide,
And then reach the effect of Stabilizing Hydrogen Peroxide.
Inventor has found that prior art at least has problems with：
The hydrogen peroxide stabilizer that prior art is provided can be adsorbed to be etched while bind metal ion
Metal surface, ultimately causes and metal residual occurs in etching products.
The content of the invention
Embodiment of the present invention technical problem to be solved is, there is provided one kind can not only make stabilized hydrogen peroxide
And will not adsorb and cause the hydrogen peroxide stabilizer of metal residual in metal surface to be etched, and by this pair
The hydrogen peroxide etching solution that oxygen water stabilizer is prepared.Concrete technical scheme is as follows：
In a first aspect, a kind of hydrogen peroxide stabilizer is the embodiment of the invention provides, in the hydrogen peroxide stabilizer
Number simultaneously containing carbon atom in alcoholic extract hydroxyl group and ehter bond, and the hydrogen peroxide stabilizer is 3-12.
Specifically, preferably, the hydrogen peroxide stabilizer is selected from EGME, diethylene glycol (DEG), diethyl two
Alcohol monomethyl ether, MMB, propandiol butyl ether, diethylene glycol monobutyl ether, DPG
At least one in butyl ether, sucrose.
Second aspect, the embodiment of the invention provides a kind of hydrogen peroxide etching solution, including effective dose is above-mentioned
Hydrogen peroxide stabilizer.
Specifically, preferably, the hydrogen peroxide etching solution includes following components in percentage by weight：
Hydrogen peroxide stabilizer 2-50%, hydrogen peroxidase 10 .5-30%, balance of water and buffer；The buffer
For the pH of the hydrogen peroxide etching solution to be adjusted to 0.5-11.
Specifically, preferably, the percentage by weight of the hydrogen peroxide stabilizer is 10-20%, the peroxide
The percentage by weight for changing hydrogen is 10-15%, and the percentage by weight of the buffer is 5-15%.
Specifically, preferably, the pH of the hydrogen peroxide etching solution is 0.5-5, for copper etching.
Specifically, preferably, the pH of the hydrogen peroxide etching solution is 5-11, for titanium or titanium alloy etching.
Specifically, preferably, the buffer is phosphoric acid, phosphate or alkali.
Specifically, preferably, the phosphate be sodium ascorbyl phosphate, potassium phosphate, ammonium phosphate salt in extremely
Few one kind.
Specifically, preferably, the alkali is NaOH and/or potassium hydroxide.
The beneficial effect that technical scheme provided in an embodiment of the present invention is brought is：
It is provided in an embodiment of the present invention with constituted above hydrogen peroxide stabilizer, use it for hydrogen peroxide system
When in metal etch liquid, its decomposition that can substantially suppress hydrogen peroxide, and using containing the hydrogen peroxide stabilizer
Etching solution be etched, the metal material surface after etching will not kish, beneficial to improve etching it is equal
One property.It can be seen that, hydrogen peroxide stabilizer provided in an embodiment of the present invention can not only improve hydrogen peroxide system etching solution
Stability in use and the shelf-life, and beneficial to ensure hydrogen peroxide system etching solution etch effect.
Specific embodiment
Unless otherwise defined, all technical terms used by the embodiment of the present invention are respectively provided with and people in the art
The identical implication that member is generally understood that.To make the object, technical solutions and advantages of the present invention clearer, under
Embodiment of the present invention is described further in detail in face.
In a first aspect, a kind of hydrogen peroxide stabilizer is the embodiment of the invention provides, it is same in the hydrogen peroxide stabilizer
The number of carbon atom is 3-12 in Shi Hanyou alcoholic extract hydroxyl groups and ehter bond, and the hydrogen peroxide stabilizer.For example,
In the hydrogen peroxide stabilizer number of carbon atom can for 3,4,5,6,7,8,9
It is individual, 10,11,12 etc..
Inventor's research finds, provided in an embodiment of the present invention with constituted above hydrogen peroxide stabilizer, by it
During in the metal etch liquid of hydrogen peroxide system, its decomposition that can substantially suppress hydrogen peroxide, and utilize
Etching solution containing the hydrogen peroxide stabilizer is etched, the metal material surface after etching will not kish,
Beneficial to the homogeneity for improving etching.It can be seen that, hydrogen peroxide stabilizer provided in an embodiment of the present invention can not only be improved
The stability in use of hydrogen peroxide system etching solution and shelf-life, and beneficial to the erosion of guarantee hydrogen peroxide system etching solution
Carve effect.
Specifically, preferably, when hydrogen peroxide stabilizer is selected from EGME, diethylene glycol (DEG), diethylene glycol
Monomethyl ether, MMB, propandiol butyl ether, diethylene glycol monobutyl ether, DPG fourth
During at least one in ether, sucrose, it has for hydrogen peroxide
Excellent stablizing effect.
On this basis, second aspect, the embodiment of the present invention additionally provides a kind of hydrogen peroxide etching solution, its bag
Include the above-mentioned hydrogen peroxide stabilizer of effective dose.It is understood that what " effective dose " described herein referred to
It is the demand under the etch effect that can guarantee that stablizing effect to hydrogen peroxide and do not interfere with hydrogen peroxide etching solution
Amount.
Specifically, the hydrogen peroxide etching solution includes following components in percentage by weight：Hydrogen peroxide stabilizer 2-50%,
Hydrogen peroxidase 10 .5-30%, balance of water and buffer.Wherein, buffer is used for the hydrogen peroxide etching solution
PH is adjusted to the amount of 0.5-11, i.e. buffer and is defined by that can meet the pH of the hydrogen peroxide etching solution.Thus may be used
To find out, its composition of hydrogen peroxide etching solution provided in an embodiment of the present invention is very simple, Environmental Safety and cost
It is cheap, have great importance for metal etch, particularly copper, titanium or titanium alloy etching.
Preferably, in the hydrogen peroxide etching solution, the percentage by weight of the hydrogen peroxide stabilizer is 10-20%,
The percentage by weight of hydrogen peroxide is 10-15%, and the percentage by weight of buffer is 5-15%, balance of water.
For example, the percentage by weight of hydrogen peroxide stabilizer can for 10%, 11%, 12%, 13%, 13%,
14%th, 15%, 16%, 17%, 18%, 19%, 20% etc.；The percentage by weight of hydrogen peroxide can be
10%th, 11%, 12%, 13%, 13%, 14%, 15% etc.；The percentage by weight of buffer is can be
5%th, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14% etc..
Research finds, for copper, titanium or titanium alloy, its etch-rate has directly pass with the pH of etching solution
System, the pH conditions needed for different metal are inconsistent.Specifically, when the pH of the hydrogen peroxide etching solution is 0.5-5
When, during preferably 1.5-3.0, it can be used for copper etching, and can reach good etch effect.When the dioxygen
When the pH of water etching solution is 5-11, during preferably 7.0-9.5, it can be used for titanium or titanium alloy etching, and energy
Reach good etch effect.
It is pH scopes as implied above that the embodiment of the present invention adjusts hydrogen peroxide etching solution by using buffer,
On this basis, in order to ensure etching solution during metal is etched, it will not be because of introducing metal ion
Cause the pH of system to fluctuate, make as far as possible etching solution etching pH stabilization, preferred reducing be phosphoric acid,
Phosphate or alkali.Specifically, phosphate is sodium ascorbyl phosphate (such as disodium hydrogen phosphate etc.), potassium phosphate
At least one in (such as potassium dihydrogen phosphate, potassium phosphate etc.), ammonium phosphate salt (such as ammonium phosphate etc.)；Alkali
It is NaOH and/or potassium hydroxide.
On the basis of being defined as above to buffer, the etch effect good in order to ensure etching solution, together
The compatibility that cooperates with of Shi Tigao and buffer, hydrogen peroxide stabilizer is preferably ethylene glycol first in the embodiment of the present invention
Ether, diethylene glycol (DEG), diethylene glycol monomethyl ether, MMB, propandiol butyl ether, diethyl two
At least one in alcohol monobutyl ether, dipropylene, sucrose.
Wherein, sucrose is referred to as sucrose by the embodiment of the present invention.
Hereinafter the present invention will be further described through by specific embodiment.It is involved in specific examples below
And the unreceipted condition person of operation, the condition advised according to normal condition or manufacturer carries out.Original used
Expect unreceipted production firm and specification person be can by city available from conventional products.
Wherein, in specific examples below, a diameter of 4 inches of wafers (are coated with 0.5um thickness
Copper), and thickness 1mm × 4cm wide × 4cm long copper coin, as copper etch raw material.By a diameter of 4
The wafer (be coated with 0.1um thick titanium) of inch, and thickness 1mm × 4cm wide × 4cm long titanium plate,
As the raw material that titanium is etched.
The hydrogen peroxide provided by using stabilizer and the present invention commonly used in the art in specific examples below
Stabilizer prepares different hydrogen peroxide etching solutions respectively, and tests each dioxygen water erosion in the following way
Carve the etch effect of liquid：
(1) stability of foundation：Each 100ml of each hydrogen peroxide etching solution to be measured is taken, 500ml is contained in
In single-necked flask, and mouthful install condenser pipe additional in each flask and open condensed water.Then each flask is all placed in
Heating, timing moment is placed in oil bath pan since flask in 50 DEG C of oil bath pan.Taken from oil bath pan after 3h
Go out flask, keep condensing unit to work on 1h afterwards, now terminate timing.While timing is terminated,
Each hydrogen peroxide etching solution sampling after to every group of cooling.And the method by permanganate titration detects that each group is lost
Carve the content of the hydrogen peroxide in liquid.
(2) stability of each hydrogen peroxide etching solution is tested after metal etch：Take each hydrogen peroxide etching solution to be measured
Each 200ml, is respectively placed in the beaker of 1L capacity, and (ready wafer then is coated with into 0.5um
The copper of thickness is coated with the titanium of 0.1um thickness) it is totally submerged in hydrogen peroxide etching solution, until wafer
On layers of copper or titanium layer be completely etched totally (for ensure copper/titanium etching quality it is identical, in each beaker
Hydrogen peroxide etching solution carries out an etching process), etching solution opening is statically placed in 25 DEG C of environmental experiment afterwards
It is indoor.By the method for permanganate titration, respectively in 0h, 24h detects etching in every group of beaker after 48h
The content of hydrogen peroxide of liquid.Wherein it is possible to understand, hydrogen peroxide (H in hydrogen peroxide etching solution2O2)
Content can be used as the whether stable direct standard of hydrogen peroxide etching solution.In following examples, with H2O2Phase
To decrement/%=H2O2Decrement/H2O2Total amount characterizes the standard of hydrogen peroxide etching solution stability to obtain.
(3) the etching homogeneity of each hydrogen peroxide etching solution is tested：By ready copper/titanium sheet, be totally submerged into
In solution to be measured, taken out after 5min, decrement calculates copper/titanium sheet corrosion rate by weight.Afterwards according to etching
The etch-rate of liquid determines the time T required for etching 0.5um copper and 0.1um titaniums, then with the etching of 1.2T
Time is etched to the metal on wafer.After taking out wafer, gold on electron microscope observation wafer is used
The revolution mark and remanent point number of category.Further judge double by observing metal residual area and residual points
The homogeneity of oxygen water etching solution, the residual degree of metal is characterized by following symbol：
Zero represents metal seriously remains>1000μm2Or>30
△ represents metal and remains remainder on a small quantity
● represent the basic noresidue of metal<100μm2And<10
The concrete composition and its etch effect of each hydrogen peroxide etching solution are distinguished as shown in Table 1 and Table 2, wherein table
Hydrogen peroxide etching solution listed in 1 is used to copper etching, and hydrogen peroxide etching solution listed in table 2 is used
In titanium etching.In addition need to give an explaination as follows：First, each dioxygen water erosion listed in Tables 1 and 2
It is 100% with water polishing percentage by weight to carve liquid, and water and its content do not show in Tables 1 and 2；Second,
Sucrose described in Tables 1 and 2 refers to sucrose；Third,
In Tables 1 and 2 in the process for preparation of listed each hydrogen peroxide etching solution, weight percent is with the addition of first
Than the disodium hydrogen phosphate for 5%, hydrogen peroxide etching solution is adjusted by buffer listed in addition table afterwards
PH for shown in table.
Table 1
Table 2
From Tables 1 and 2, by comparative example 1 and embodiment 1, comparative example 5 and embodiment 8, than
Compared with example 6 and embodiment 9, comparative example 11 and the essentially identical hydrogen peroxide of this four groups of pH value of embodiment 18 are etched
Liquid, it is known that hydrogen peroxide stabilizer provided in an embodiment of the present invention can effectively reduce decomposing hydrogen dioxide solution speed.By
It is above-mentioned to understand, compared to producing hydrogen peroxide etching solution is matched somebody with somebody using the conventional hydrogen peroxide stabilizer of prior art, utilize
Come the hydrogen peroxide etching solution prepared, it can effectively reduce double to hydrogen peroxide stabilizer provided in an embodiment of the present invention
The decomposition rate of oxygen water, the effectively Stabilizing Hydrogen Peroxide in etching process keeps the original of hydrogen peroxide etching solution
Etching environment.Additionally, while Stabilizing Hydrogen Peroxide effect is reached, using the hydrogen peroxide of common stabilizer
Etching solution has a metal residual after being susceptible to etching, and hydrogen peroxide etching solution provided in an embodiment of the present invention not shadow
Metal etch performance is rung, preferably etching homogeneity is maintained.
Presently preferred embodiments of the present invention is the foregoing is only, the protection domain being not intended to limit the invention is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements made etc., all should include
Within protection scope of the present invention.
Claims (10)
1. a kind of hydrogen peroxide stabilizer, it is characterised in that contain alcoholic extract hydroxyl group simultaneously in the hydrogen peroxide stabilizer
And the number of carbon atom is 3-12 in ehter bond, and the hydrogen peroxide stabilizer.
2. hydrogen peroxide stabilizer according to claim 1, it is characterised in that the hydrogen peroxide stabilizer
Selected from EGME, diethylene glycol (DEG), diethylene glycol monomethyl ether, MMB, propane diols
Butyl ether, diethylene glycol monobutyl ether, dipropylene, sucrose
In at least one.
3. a kind of hydrogen peroxide etching solution, including the hydrogen peroxide stabilizer described in the claim 1 or 2 of effective dose.
4. hydrogen peroxide etching solution according to claim 3, it is characterised in that the hydrogen peroxide etching solution
Including following components in percentage by weight：
Hydrogen peroxide stabilizer 2-50%, hydrogen peroxidase 10 .5-30%, balance of water and buffer；The buffer
For the pH of the hydrogen peroxide etching solution to be adjusted to 0.5-11.
5. hydrogen peroxide etching solution according to claim 4, it is characterised in that the hydrogen peroxide stabilizer
Percentage by weight be 10-20%, the percentage by weight of the hydrogen peroxide is 10-15%, the buffer
Percentage by weight is 5-15%.
6. hydrogen peroxide etching solution according to claim 4, it is characterised in that the hydrogen peroxide etching solution
PH be 0.5-5, for copper etching.
7. hydrogen peroxide etching solution according to claim 4, it is characterised in that the hydrogen peroxide etching solution
PH be 5-11, for titanium or titanium alloy etching.
8. the hydrogen peroxide etching solution according to claim any one of 4-7, it is characterised in that the buffering
Agent is phosphoric acid, phosphate or alkali.
9. hydrogen peroxide etching solution according to claim 8, it is characterised in that the phosphate is phosphoric acid
At least one in sodium salt, potassium phosphate, ammonium phosphate salt.
10. hydrogen peroxide etching solution according to claim 8, it is characterised in that the alkali is hydroxide
Sodium and/or potassium hydroxide.
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| CN201510937359.6A CN106884167A (en) | 2015-12-15 | 2015-12-15 | A kind of hydrogen peroxide stabilizer and hydrogen peroxide etching solution |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107604362A (en) * | 2017-09-14 | 2018-01-19 | 江阴江化微电子材料股份有限公司 | A kind of two-component selectivity titanium corrosive liquid and titanium caustic solution |
| CN108203828A (en) * | 2018-01-09 | 2018-06-26 | 东莞市耀辉化工科技有限公司 | A kind of environmentally friendly hanger stripper of wiring board nitre hanger |
| CN109321957A (en) * | 2018-10-24 | 2019-02-12 | 中国电子科技集团公司第五十五研究所 | A kind of environment-friendly type shell plating pre-treatment etching solution technique and coating method |
| CN109628934A (en) * | 2018-08-30 | 2019-04-16 | 上海昕沐化学科技有限公司 | Environment-friendly type takes off tin liquor and preparation method thereof |
| CN109652803A (en) * | 2018-12-28 | 2019-04-19 | 太仓市何氏电路板有限公司 | Protect etching solution in a kind of LED aluminium face |
| CN111074330A (en) * | 2019-12-07 | 2020-04-28 | 西北有色金属研究院 | TiAl-series medical titanium alloy implant surface micropore preparation method |
| CN112522707A (en) * | 2020-11-20 | 2021-03-19 | 湖北兴福电子材料有限公司 | Tungsten etching solution with high selectivity ratio |
| CN112981405A (en) * | 2021-02-23 | 2021-06-18 | 江苏艾森半导体材料股份有限公司 | Titanium-tungsten etching solution and preparation method and application thereof |
| CN113445052A (en) * | 2021-07-28 | 2021-09-28 | 南通群安电子材料有限公司 | Differential etching solution suitable for MSAP (multiple-site-sensitive protection) process |
| CN113529085A (en) * | 2021-07-15 | 2021-10-22 | 深圳市华星光电半导体显示技术有限公司 | Etching solution and etching method |
| CN114107989A (en) * | 2020-08-31 | 2022-03-01 | 深圳新宙邦科技股份有限公司 | Etching solution for copper-containing metal film |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107604362A (en) * | 2017-09-14 | 2018-01-19 | 江阴江化微电子材料股份有限公司 | A kind of two-component selectivity titanium corrosive liquid and titanium caustic solution |
| CN108203828A (en) * | 2018-01-09 | 2018-06-26 | 东莞市耀辉化工科技有限公司 | A kind of environmentally friendly hanger stripper of wiring board nitre hanger |
| CN109628934A (en) * | 2018-08-30 | 2019-04-16 | 上海昕沐化学科技有限公司 | Environment-friendly type takes off tin liquor and preparation method thereof |
| CN109628934B (en) * | 2018-08-30 | 2021-04-16 | 上海昕沐化学科技有限公司 | Environment-friendly tin removing liquid and preparation method thereof |
| CN109321957A (en) * | 2018-10-24 | 2019-02-12 | 中国电子科技集团公司第五十五研究所 | A kind of environment-friendly type shell plating pre-treatment etching solution technique and coating method |
| CN109321957B (en) * | 2018-10-24 | 2023-01-17 | 中国电子科技集团公司第五十五研究所 | Environment-friendly shell plating pretreatment etching solution process and plating method |
| CN109652803A (en) * | 2018-12-28 | 2019-04-19 | 太仓市何氏电路板有限公司 | Protect etching solution in a kind of LED aluminium face |
| CN111074330A (en) * | 2019-12-07 | 2020-04-28 | 西北有色金属研究院 | TiAl-series medical titanium alloy implant surface micropore preparation method |
| CN111074330B (en) * | 2019-12-07 | 2021-04-02 | 西北有色金属研究院 | TiAl-series medical titanium alloy implant surface micropore preparation method |
| CN114107989A (en) * | 2020-08-31 | 2022-03-01 | 深圳新宙邦科技股份有限公司 | Etching solution for copper-containing metal film |
| CN112522707A (en) * | 2020-11-20 | 2021-03-19 | 湖北兴福电子材料有限公司 | Tungsten etching solution with high selectivity ratio |
| CN112981405A (en) * | 2021-02-23 | 2021-06-18 | 江苏艾森半导体材料股份有限公司 | Titanium-tungsten etching solution and preparation method and application thereof |
| CN113529085A (en) * | 2021-07-15 | 2021-10-22 | 深圳市华星光电半导体显示技术有限公司 | Etching solution and etching method |
| CN113445052A (en) * | 2021-07-28 | 2021-09-28 | 南通群安电子材料有限公司 | Differential etching solution suitable for MSAP (multiple-site-sensitive protection) process |
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Application publication date: 20170623 |