CN101799381A - Method for forming oxide layer on surface of silicon wafer - Google Patents
Method for forming oxide layer on surface of silicon wafer Download PDFInfo
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- CN101799381A CN101799381A CN 201010116252 CN201010116252A CN101799381A CN 101799381 A CN101799381 A CN 101799381A CN 201010116252 CN201010116252 CN 201010116252 CN 201010116252 A CN201010116252 A CN 201010116252A CN 101799381 A CN101799381 A CN 101799381A
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Abstract
A method for forming an oxide layer on the surface of silicon wafer comprises the following steps: (a) washing the silicon wafer to be detected with hydrofluoric acid solution with the mass concentration of 15% to 17%, wherein the washing lasts 20-40s; (b) rinsing the silicon wafer to be detected with deionized water; (c) washing the silicon wafer to be detected with hydrogen peroxide solution with the mass concentration of 8%-12% and at the temperature of 70-90 DEG C, wherein the washing lasts 60-100s; (d) rinsing the silicon wafer to be detected with deionized water; and (e) drying the silicon wafer to be detected with nitrogen gas. The method has the advantages of saving time and technological cost by optimizing the concentrations of hydrofluoric acid and hydrogen peroxide and the washing time.
Description
[technical field]
The present invention relates to the semiconductor material field tests, relate in particular to a kind of method that forms oxide layer at silicon chip surface.
[background technology]
In recent years along with the continuous expansion of silicon epitaxial wafer large-scale production, taking on a very important role as capacitance-voltage (CV) method of testing of the classical method of testing of epitaxial wafer resistivity measurement.The CV method is a kind of measurement pattern by providing scanning voltage to obtain capacitance parameter, adopts specific formula conversion method capacitance parameter to be converted to the method for testing of sample resistivity data then.The pre-service of test pieces is a requisite step in the CV test.Disposal route to test pieces in the prior art is to adopt the method for " hydrofluorite-hydrogen peroxide " Combined Treatment that silicon chip is carried out pre-service, forms a compact oxide with the surface at silicon slice under test.Specifically, this method comprises the steps:
Step S11 adopts hydrofluoric acid solution to remove the natural oxidizing layer of silicon slice under test surface porosity, and the concentration of the hydrofluoric acid solution that is adopted is 4.9% (weight), and scavenging period is 30 seconds;
Step S12 adopted the deionized water rinsing silicon slice under test 10 minutes, to remove the remaining hydrofluoric acid solution in silicon slice under test surface;
Step S13, adopting concentration is 15% (weight), temperature is that 70 ℃ to 90 ℃ hydrogen peroxide solution cleaned silicon slice under test 10 minutes, to form one deck compact oxide on the silicon slice under test surface, this oxide layer is mainly used in carries out follow-up CV test, because hydrogen peroxide is a kind of strong oxidizer, therefore adopt hydrogen peroxide to handle the oxide layer quality densification that forms, can be used for the CV test, the oxide layer that forms naturally in air then quality is loose, can not be used for test;
Step S14 adopted the deionized water rinsing silicon slice under test 2 minutes, to remove the remaining hydrogen peroxide solution in silicon slice under test surface;
Step S15 adopts nitrogen to dry up silicon slice under test.
Though test repeated aspect still can, shortcoming is that the time of handling is long, above technology total consuming time is at least 22 minutes 30 seconds (do not comprise that still silicon slice under test circulates the required time between each step, and nitrogen drying up the spent time).For the industrial applications of producing in batches, if every day, turnout was very big, then need the quantity of test pieces also very huge, tediously long disposal route does not just catch up with the requirement of real-time production to speed in the prior art so.
[summary of the invention]
Technical matters to be solved by this invention is, provides a kind of and forms the method for oxide layer at silicon chip surface, can shorten the process time, to satisfy the requirement of actual production to process speed.
In order to address the above problem, the invention provides a kind of method of handling silicon chip surface, comprise the steps: that (a) adopts mass concentration is 15% to 17%, be preferably 16% hydrofluoric acid solution cleaning silicon slice under test, to remove the natural oxidizing layer of silicon slice under test surface porosity, scavenging period is 20 to 40 seconds, is preferably 30 seconds; (b) adopt the deionized water rinsing silicon slice under test, to remove the remaining hydrofluoric acid solution in silicon slice under test surface; (c) adopting mass concentration is 8% to 12%, is preferably 10%, and temperature is that 70 ℃ to 90 ℃ hydrogen peroxide solution cleans silicon slice under test, and scavenging period is 60 to 100 seconds, is preferably 90 seconds, to form one deck compact oxide on the silicon slice under test surface; (d) adopt the deionized water rinsing silicon slice under test, to remove the remaining hydrogen peroxide solution in silicon slice under test surface; (e) adopt nitrogen to dry up silicon slice under test.
As optional technical scheme, in the described step (b), adopting the time of deionized water rinsing silicon slice under test is 1 to 3 minute, is preferably 2 minutes.
As optional technical scheme, in the described step (d), adopting the time of deionized water rinsing silicon slice under test is 1 to 3 minute, is preferably 2 minutes.
As optional technical scheme, in the described step (e), the time that nitrogen dries up is 40 seconds to 2 minutes, is preferably 1 minute.
As optional technical scheme, in the described step (c), adopt the method for water-bath heating that hydrogen peroxide is heated to required temperature.
The invention has the advantages that, by optimizing the concentration and the scavenging period of hydrofluorite and hydrogen peroxide, reached the purpose that saves time with the technology cost.Further optimize the time of washed with de-ionized water, can shorten the required time of whole technologies more.
[description of drawings]
It shown in the accompanying drawing 1 the implementation step synoptic diagram of embodiment of the present invention.
[embodiment]
Below in conjunction with accompanying drawing a kind of embodiment that forms the method for oxide layer at silicon chip surface provided by the invention is elaborated.
Accompanying drawing 1 is depicted as the implementation step synoptic diagram of the method for the invention embodiment, comprising: step S11, and the employing mass concentration is 15%～17% hydrofluoric acid solution cleaning silicon slice under test, scavenging period is not more than 30 seconds; Step S12 adopts the deionized water rinsing silicon slice under test; Step S13, adopting mass concentration is 8%～12%, and temperature is that 70 ℃～90 ℃ hydrogen peroxide solution cleans silicon slice under test, and scavenging period is not more than 90 seconds; Step S14 adopts the deionized water rinsing silicon slice under test, to remove the remaining hydrogen peroxide solution in silicon slice under test surface; Step S15 adopts nitrogen to dry up silicon slice under test.
The purpose of the described method of this embodiment is to show formation one deck compact oxide by cleaning at silicon chip, so that subsequent implementation CV test.
Refer step S11 at first, adopting mass concentration is that 15%～17% hydrofluoric acid solution cleans silicon slice under test, scavenging period is not more than 30 seconds.The effect of this step is to remove the natural oxidizing layer of silicon slice under test surface porosity, and the oxide layer quality that this forms naturally is loose, is not suitable for the requirement of follow-up CV test to surface oxide layer, therefore will at first adopt hydrofluoric acid solution that its corrosion is removed.The mass concentration of the hydrofluorite that is adopted is 15%～17%, and is preferably 16%.Under this concentration, scavenging period is 20 to 40 seconds, and is preferably 30 seconds.Experiment shows, under this concentration and time conditions, the oxide layer on silicon slice under test surface can be removed fully.Than the hydrofluorite of available technology adopting 49%, this embodiment can be saved the consumption of hydrofluorite in this step, reduces the technology cost.
Refer step S12 adopts the deionized water rinsing silicon slice under test again, to remove the remaining hydrofluoric acid solution in silicon slice under test surface.Will have influence on normally carrying out of follow-up test because the hydrofluorite during previous step is rapid remains in the surface of silicon slice under test, therefore need to adopt deionized water that the hydrofluoric acid clean on surface is removed.Prior art also is this cleaning to be done to study in great detail see, and generally adopts 10 minutes scavenging period.This embodiment is because the hydrofluoric acid concentration that adopted is low than prior art, thus the corresponding cleaning time promptly can adopt 10 minutes conventional clean time, also can reduce scavenging period accordingly.Experiment shows that adopting the time of deionized water rinsing silicon slice under test is 1～3 minute, is preferably 2 minutes, just can be with the whole flush awaies of the hydrofluorite on surface.
Refer step S13 again, adopting mass concentration is 8%～12%, and temperature is that 70 ℃～90 ℃ hydrogen peroxide solution cleans silicon slice under test, and scavenging period is 60 to 100 seconds.The purpose of this step is to form one deck compact oxide on the silicon slice under test surface.Because hydrogen peroxide is a strong oxidizer, therefore the compactness extent in the formed oxide layer in silicon slice under test surface will can satisfy the demand of CV test much larger than the oxide layer density that forms naturally in air.Experiment shows that adopting mass concentration is 8%～12%, is preferably 10%, temperature is 70 ℃～90 ℃ a hydrogen peroxide, only needs 60 to 100 seconds time, and is preferably 90 seconds, can form compact oxide on the surface of silicon slice under test, save about 500 seconds time than prior art.
Further, because hydrogen peroxide is a kind of strong oxidizer, at high temperature use the hydrogen peroxide of high concentration bring potential danger can for operating personnel and line of production technology for a long time.The hydrogen peroxide concentration that this embodiment adopted is low than prior art, the also corresponding shortening of scavenging period, thus reduced the danger of using hydrogen peroxide to bring owing to long-time.Adopt the method for water-bath heating that hydrogen peroxide is heated to required temperature, than direct-fired method, the process of its heating more relaxes, and hydrogen peroxide is thermally equivalent in container, can not produce phenomenons such as splash owing to local overheating, help improving the security of technological operation more.
At refer step S14, adopt the deionized water rinsing silicon slice under test.The purpose of this step is to remove the remaining hydrogen peroxide solution in silicon slice under test surface.Because the scavenging period that is adopted during previous step is rapid is shorter, therefore the time with the deionized water rinsing silicon slice under test is 1～3 minute, is preferably 2 minutes, just can be with the whole flush awaies of the hydrogen peroxide on surface.
At refer step S15, adopt nitrogen to dry up silicon slice under test.The time to this step is not made optimization in the prior art.The time that dries up of being adopted in this embodiment is 40 seconds to 2 minutes, and is preferably 1 minute.
The described method of this embodiment has been saved the process time than prior art, and has improved process safety.
Next provide an embodiment:
Step 1, N type test pieces was soaked 30 seconds in the hydrofluorite of concentration 16%;
Step 2 is used pure water rinsing 2 minutes;
Step 3 is transferred to test pieces in hydrogen peroxide (concentration 10%) soup of water-bath (80 degrees centigrade) heating and soaked 90 seconds;
Step 4 was with pure water rinsing flushing 2 minutes;
Step 5 dries up 1 minute with nitrogen.
Said method has been saved about 20 minutes time than prior art.After tested, for the silicon chip of identical 1ohm.cm, carry out the CV test after employing prior art and said method are handled, the result has higher consistance, and deviation only is 1.37%.
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. a method of handling silicon chip surface is characterized in that, comprises the steps:
(a) the employing mass concentration is 15% to 17% hydrofluoric acid solution cleaning silicon slice under test, and to remove the natural oxidizing layer of silicon slice under test surface porosity, scavenging period is 20 to 40 seconds;
(b) adopt the deionized water rinsing silicon slice under test, to remove the remaining hydrofluoric acid solution in silicon slice under test surface;
(c) adopting mass concentration is 8% to 12%, and temperature is that 70 ℃ to 90 ℃ hydrogen peroxide solution cleans silicon slice under test, and scavenging period is 60 to 100 seconds, to form one deck compact oxide on the silicon slice under test surface;
(d) adopt the deionized water rinsing silicon slice under test, to remove the remaining hydrogen peroxide solution in silicon slice under test surface;
(e) adopt nitrogen to dry up silicon slice under test.
2. method according to claim 1 is characterized in that, in the described step (b), adopting the time of deionized water rinsing silicon slice under test is 1 to 3 minute.
3. method according to claim 1 is characterized in that, in the described step (d), adopting the time of deionized water rinsing silicon slice under test is 1 to 3 minute.
4. method according to claim 1 is characterized in that, in the described step (e), the time that nitrogen dries up is 40 seconds to 2 minutes.
5. method according to claim 1 is characterized in that, in the described step (c), adopts the method for water-bath heating that hydrogen peroxide is heated to required temperature.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102231404A (en) * | 2011-05-20 | 2011-11-02 | 浙江星宇能源科技有限公司 | Technology for cleaning solar monocrystalline wafer |
| WO2013026277A1 (en) * | 2011-08-19 | 2013-02-28 | 上海新傲科技股份有限公司 | Preparation method of multilayer semiconductor substrate |
| CN103681241A (en) * | 2013-12-18 | 2014-03-26 | 无锡中微晶园电子有限公司 | Cleaning method capable of improving quality of oxide layer |
| CN105334096A (en) * | 2015-11-04 | 2016-02-17 | 浙江理工大学 | Method for performing strontium element enrichment on silk fabric cultural relics |
| CN107256837A (en) * | 2017-07-19 | 2017-10-17 | 河北普兴电子科技股份有限公司 | The measuring method of the electrical resistivity of substrate is sealed based on the super back of the body |
| CN112485090A (en) * | 2020-12-03 | 2021-03-12 | 西安奕斯伟硅片技术有限公司 | Method for testing copper content of silicon wafer |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102231404A (en) * | 2011-05-20 | 2011-11-02 | 浙江星宇能源科技有限公司 | Technology for cleaning solar monocrystalline wafer |
| WO2013026277A1 (en) * | 2011-08-19 | 2013-02-28 | 上海新傲科技股份有限公司 | Preparation method of multilayer semiconductor substrate |
| CN103681241A (en) * | 2013-12-18 | 2014-03-26 | 无锡中微晶园电子有限公司 | Cleaning method capable of improving quality of oxide layer |
| CN105334096A (en) * | 2015-11-04 | 2016-02-17 | 浙江理工大学 | Method for performing strontium element enrichment on silk fabric cultural relics |
| CN107256837A (en) * | 2017-07-19 | 2017-10-17 | 河北普兴电子科技股份有限公司 | The measuring method of the electrical resistivity of substrate is sealed based on the super back of the body |
| CN107256837B (en) * | 2017-07-19 | 2020-01-07 | 河北普兴电子科技股份有限公司 | Method for measuring resistivity of epitaxial wafer based on super back-sealed substrate |
| CN112485090A (en) * | 2020-12-03 | 2021-03-12 | 西安奕斯伟硅片技术有限公司 | Method for testing copper content of silicon wafer |
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| CN101799381B (en) | 2012-03-14 |
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