CN109904089A - A kind of test method measuring wafer bulk metal - Google Patents

A kind of test method measuring wafer bulk metal Download PDF

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Publication number
CN109904089A
CN109904089A CN201910104745.5A CN201910104745A CN109904089A CN 109904089 A CN109904089 A CN 109904089A CN 201910104745 A CN201910104745 A CN 201910104745A CN 109904089 A CN109904089 A CN 109904089A
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China
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full
collection system
test method
silicon wafer
metal
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CN201910104745.5A
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Chinese (zh)
Inventor
刘九江
刘顺玲
李诺
谭咏麟
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Tianjin Zhonghuan Semiconductor Joint Stock Co Ltd
Tianjin Zhonghuan Advanced Material Technology Co Ltd
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Tianjin Zhonghuan Semiconductor Joint Stock Co Ltd
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Abstract

The present invention provides a kind of test methods for measuring wafer bulk metal, belong to field of semiconductor manufacture, including step 1: take 4~10inch of diameter and the unconfined silicon wafer of resistivity 1;Step 2: silicon wafer, which is uploaded to infrared heating furnace, is warming up to 200~300 degree, constant temperature is toasted 1.5~2.5 hours;Step 3: silicon wafer is uploaded to full-automatic surface metal collection system;Step 4: full-automatic surface metal collection system blows hydrofluoric acid vapor 4~6 minutes to silicon chip surface in sample making course;Step 5: the nozzle of full-automatic surface metal collection system draws extracting solution, metal ion is recycled in silicon chip surface;Step 6: testing scanning liquid tenor using Inductively coupled plasma mass spectrometry, the surface metal levels tested out pass through the metal ion spill-out of infrared heating furnace baking.There is no limit test scope is wider, and precision is higher, and cost is lower for silicon wafer diameter and resistivity of the present invention to test.

Description

A kind of test method measuring wafer bulk metal
Technical field
The invention belongs to field of semiconductor manufacture, are related to a kind of test method for measuring wafer bulk metal.
Background technique
Semiconductor manufacturing industry wafer bulk metallic test is difficult, and cost is excessively high when body metallic test, scans when testing heavily doped silicon wafer Liquid can not recycle, and large-diameter silicon wafer is unable to test, and due to the more wasteful time, can not accomplish asking for the daily monitoring of body metal Topic.Traditional test mode is corroded using ozone+hydrofluoric acid vapor, recycles metal ion on corrosion of silicon surface, Using silicon wafer weight after high accuracy balance record corrosion, and corrosion volume is calculated by the difference of weight, inductive coupling etc. from Sub- mass spectrograph test scanning liquid tenor, thus according to ozone+hydrofluoric acid vapor (HF+O3) volume that erodes and surface gold Belonging to ion concentration and calculates metal ion content in silicon wafer unit volume, traditional test method has the following disadvantages, 1, by day Flat volume influences, and cannot test large-diameter silicon wafer;2, it is influenced by by roughness after corroding, as 1 Ω .cm of silicon chip resistivity <, Inductively coupled plasma mass spectrometry can not recycle scanning liquid, be unable to test;3, cost when a piece of 6 inch silicon wafer of test is 251.53 yuan/piece, higher cost;4, it can not be used as the monitoring of daily body metal by time-constrain.
Summary of the invention
The problem to be solved in the present invention is to be to provide a kind of test method for measuring wafer bulk metal, to the silicon wafer of test There is no limit test scope is wider, and precision is higher, and cost is lower for diameter and resistivity.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of test side measuring wafer bulk metal Method includes the following steps,
Step 1: taking 4~10inch of diameter and the unconfined silicon wafer of resistivity 1;
Step 2: silicon wafer described in the first step, which is uploaded to infrared heating furnace, is warming up to 200~300 degree, constant temperature baking 1.5~2.5 hours;
Step 3: the silicon wafer is uploaded to full-automatic surface metal collection system on the basis of second step is completed;
Step 4: the full-automatic surface metal collection system blows hydrofluoric acid vapor 4 to silicon chip surface in sample making course ~6 minutes;
Step 5: the nozzle of the full-automatic surface metal collection system draws extracting solution, metal is recycled in silicon chip surface Ion;
Step 6: testing scanning liquid tenor using Inductively coupled plasma mass spectrometry, the surface metal tested out contains Metal ion spill-out of the amount i.e. by infrared heating furnace baking.
Further, in the first step, the diameter of the silicon wafer is 5inch, 6inch or 8inch.
Further, in the second step, the infrared heating furnace is warming up to 250 ± 3 degree, and constant temperature toasts 2 hours.
Further, in the 4th step, hydrofluoric acid vapor is blown 5 minutes to silicon chip surface, flow 180ul/min, The nozzle of the full-automatic surface metal collection system draws 1000ul extracting solution.
Further, the proportion of the extracting solution is 0.3%HF+11.4%H2O2+ 88.28%H2O, HF (hydrofluoric acid) are dense Degree: 38% Japan chemical AA-10 purity of rubbing, H more2O2(hydrogen peroxide) concentration: 35% Japan chemical AA-10 purity of rubbing, H more2O is (super Pure water): resistivity >=18M Ω .cm.
Further, after the completion of second step, 23 ± 2 degree are cooled to, when silicon chip surface reaches room temperature, is inhaled using vacuum Silicon chip extracting is uploaded to full-automatic surface metal collection system by pen.
Further, from the first step to the 6th step, test environment is hundred grades of toilets, and room temperature is 23 ± 2 degree.
Further, in the third step, the full-automatic surface metal collection system is Beijing Qinghe Zhi Ce company The full-automatic surface metal collection system of production, in the 6th step, Inductively coupled plasma mass spectrometry Agilent 7700s Inductively coupled plasma mass spectrometry.
Compared with prior art, the present invention has the advantage that as follows with good effect.
1, for silicon wafer diameter without limitation, 5/6/8inch silicon wafer can be tested the present invention, not coarse by silicon chip surface Degree influences, and completely, test result is more accurate for the recycling of scanning liquid;
2, testing cost is greatly reduced, 106.81 yuan/piece is down to by 251.31 yuan/piece, in sample making course, is not take up Full-automatic surface metal collection system time, and the method that can be used as long-term monitoring wafer bulk metal uses;
3, it is operated in strict accordance with above step, simple and convenient, high-efficient, reliable and stable, save the cost, sample making course When being not take up automatic sample-making system machine, accurate testing is required silicon slice under test size lower.
Detailed description of the invention
The attached drawing for constituting a part of the invention is used to provide further understanding of the present invention, schematic reality of the invention It applies example and its explanation is used to explain the present invention, do not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is the test result figure that the present invention carries out two panels silicon wafer using a kind of test method for measuring wafer bulk metal.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase Mutually combination.
In the description of the present invention, it is to be understood that, term " center ", " longitudinal direction ", " transverse direction ", "upper", "lower", The orientation or positional relationship of the instructions such as "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside" is Relative bearing or positional relationship, are merely for convenience of description of the present invention and simplification of the description, rather than the dress of indication or suggestion meaning It sets or element must have a particular orientation, be constructed and operated in a specific orientation, therefore should not be understood as to limit of the invention System.In addition, term " first ", " second " etc. be used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance or Person implicitly indicates the quantity of indicated technical characteristic.Define as a result, " first ", " second " etc. feature can express or Implicitly include one or more of the features.In the description of the present invention, unless otherwise indicated, the meaning of " plurality " is two It is a or more than two.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected;It can To be mechanical connection, it is also possible to be electrically connected;It can be directly connected, can also can be indirectly connected through an intermediary Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood by concrete condition Concrete meaning in the present invention.
It elaborates below to specific embodiments of the present invention.
The present invention is a kind of test method for measuring wafer bulk metal, is included the following steps,
Step 1: taking 4~10inch of diameter and the unconfined silicon wafer of resistivity 1;
Step 2: the silicon wafer in the first step, which is uploaded to infrared heating furnace, is warming up to 200~300 degree, constant temperature baking 1.5~ 2.5 hour;
Step 3: silicon wafer is uploaded to full-automatic surface metal collection system on the basis of second step is completed;
Step 4: full-automatic surface metal collection system blows 4~6 points of hydrofluoric acid vapor to silicon chip surface in sample making course Clock;
Step 5: the nozzle of full-automatic surface metal collection system draws extracting solution, metal ion is recycled in silicon chip surface;
Step 6: testing scanning liquid tenor using Inductively coupled plasma mass spectrometry, the surface metal tested out contains Metal ion spill-out of the amount i.e. by infrared heating furnace baking.
Preferably, in the first step, the diameter of silicon wafer is 5inch, 6inch or 8inch.
Preferably, in second step, infrared heating furnace is warming up to 250 ± 3 degree, and constant temperature toasts 2 hours, 250 degree of enough silicon Energy needed for the internal metal ion of piece transits to surface, the purpose of constant temperature 2h are to transit to in-vivo metal as much as possible Silicon chip surface.
Preferably, in the 4th step, hydrofluoric acid vapor is blown 5 minutes to silicon chip surface, flow 180ul/min, daily silicon One layer of very thin silicon dioxide film can all occur in silicon chip surface behind piece surface and heating, and the thickness of this film probably existsWith It is interior, and silica, it can only react with few part acid, thus be dissolved, and this structure will use a large amount of hydrogen fluorine just Acid vapor as cleaning agent, then thisThe silicon dioxide film of left and right thickness is in 5min enough by 38% high-pure hydrofluoric acid It dissolves, the nozzle absorption 1000ul extracting solution of full-automatic surface metal collection system, ul=microlitres, 1ml=1000 ul.
Preferably, the proportion of extracting solution is 0.3%HF+11.4%H2O2+ 88.28%H2O, HF (hydrofluoric acid) concentration: 38% Japanese chemical AA-10 purity of rubbing easily is evaporated more using high concentration, and nebulization efficiency is high, and speed is fast, will not cause to damage to silicon wafer, H2O2(hydrogen peroxide) concentration: chemical AA-10 purity of rubbing 35% Japan, metal ion content control contained by solution inside exist more Within 10ppt, i.e., 10 receive within grams per liter, the pure water concentration used lower than full-automatic sample-preparing system (VPD), it is possible to meet Testing requirement avoids the impurity effect test result contained in water, promotes the accuracy of test structure, H2O (ultrapure water): resistance Rate >=18M Ω .cm, pure water are insulators, and why conductive water used in life is, are because containing mineral in water The conductors such as matter, metal ion illustrate that water is purer so the resistance value of water is higher (resistivity is lower), avoid containing in water Impurity effect test result promotes the accuracy of test structure.
Preferably, after the completion of second step, 23 ± 2 degree are cooled to, when silicon chip surface reaches room temperature, uses vacuum WAND By silicon chip extracting, it is uploaded to full-automatic surface metal collection system, using vacuum WAND, silicon wafer will not be caused to damage, also not Impurity can be infected with.
Preferably, from the first step to the 6th step, test environment is hundred grades of toilets, and room temperature is 23 ± 2 degree, and following table is environment Indoor particle test result.
Particle diameter (um) Target (a) Practical (a)
0.3 300 82
0.5 100 10
Preferably, in the third step, full-automatic surface metal collection system be the production of Beijing Qinghe Zhi Ce company it is complete from Dynamic surface metal collection system, in step 6, Inductively coupled plasma mass spectrometry Agilent 7700s inductively coupled plasma matter Spectrometer.
As shown in Figure 1, same method test samples the 2nd silicon wafer with basket, it can be seen that this test method has preferable Stability, the above structure is simple, easily operated, safe and reliable, and save the cost, sample making course are not take up automatic sample-making system machine When, accurate testing requires silicon slice under test size lower.
One embodiment of the present invention has been described in detail above, but the content is only preferable implementation of the invention Example, should not be considered as limiting the scope of the invention.It is all according to all the changes and improvements made by the present patent application range Deng should still be within the scope of the patent of the present invention.

Claims (8)

1. a kind of test method for measuring wafer bulk metal, it is characterised in that: include the following steps,
Step 1: taking 4~10inch of diameter and the unconfined silicon wafer of resistivity 1;
Step 2: silicon wafer described in the first step, which is uploaded to infrared heating furnace, is warming up to 200~300 degree, constant temperature baking 1.5~ 2.5 hour;
Step 3: the silicon wafer is uploaded to full-automatic surface metal collection system on the basis of second step is completed;
Step 4: the full-automatic surface metal collection system blows 4~6 points of hydrofluoric acid vapor to silicon chip surface in sample making course Clock;
Step 5: the nozzle of the full-automatic surface metal collection system draws extracting solution, metal ion is recycled in silicon chip surface;
Step 6: testing scanning liquid tenor using Inductively coupled plasma mass spectrometry, the surface metal levels tested out are i.e. The metal ion spill-out toasted by infrared heating furnace.
2. a kind of test method for measuring wafer bulk metal according to claim 1, it is characterised in that: in the first step In, the diameter of the silicon wafer is 5inch, 6inch or 8inch.
3. a kind of test method for measuring wafer bulk metal according to claim 1, it is characterised in that: in the second step In, the infrared heating furnace is warming up to 250 ± 3 degree, and constant temperature toasts 2 hours.
4. a kind of test method for measuring wafer bulk metal according to claim 1, it is characterised in that: in the 4th step In, hydrofluoric acid vapor is blown 5 minutes to silicon chip surface, flow 180ul/min, the spray of the full-automatic surface metal collection system Mouth draws 1000ul extracting solution.
5. a kind of test method for measuring wafer bulk metal according to claim 1, it is characterised in that: the extracting solution Proportion is 0.3%HF+11.4%H2O2+ 88.28%H2O, HF (hydrofluoric acid) concentration: 38% Japan chemical AA-10 purity of rubbing more, H2O2(hydrogen peroxide) concentration: 35% Japan chemical AA-10 purity of rubbing, H more2O (ultrapure water): resistivity >=18M Ω .cm.
6. a kind of test method for measuring wafer bulk metal according to claim 1, it is characterised in that: completed in second step Afterwards, 23 ± 2 degree are cooled to, when silicon chip surface reaches room temperature, using vacuum WAND by silicon chip extracting, is uploaded to full-automatic surface Metal collection system.
7. a kind of test method for measuring wafer bulk metal according to claim 1, it is characterised in that: from the first step To the 6th step, test environment is hundred grades of toilets, and room temperature is 23 ± 2 degree.
8. the method for the test method using a kind of measurement wafer bulk metal described in claim 1, it is characterised in that: described In third step, the full-automatic surface metal collection system is the full-automatic surface metal collection of Beijing Qinghe Zhi Ce company production System, in the 6th step, Inductively coupled plasma mass spectrometry Agilent 7700s Inductively coupled plasma mass spectrometry.
CN201910104745.5A 2019-02-01 2019-02-01 A kind of test method measuring wafer bulk metal Pending CN109904089A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112683988A (en) * 2020-12-28 2021-04-20 上海新昇半导体科技有限公司 Method for detecting metal impurities in wafer
CN112713103A (en) * 2021-03-29 2021-04-27 西安奕斯伟硅片技术有限公司 Method for measuring metal content in silicon wafer
CN113130366A (en) * 2021-03-17 2021-07-16 江苏鲁汶仪器有限公司 Nozzle for wafer scanning and system and application thereof
CN114459946A (en) * 2022-01-29 2022-05-10 西安奕斯伟材料科技有限公司 Method and equipment for testing metal content of silicon wafer
WO2023284205A1 (en) * 2021-07-16 2023-01-19 江苏鲁汶仪器有限公司 Online sampler and contamination analysis system
CN117168942A (en) * 2023-11-01 2023-12-05 山东有研艾斯半导体材料有限公司 Sampling method for detecting metal on surface of silicon wafer

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CN102980938A (en) * 2012-12-03 2013-03-20 天津中环领先材料技术有限公司 Method for testing metal ions on surface of wafer of solar battery
CN106841364A (en) * 2015-12-03 2017-06-13 有研半导体材料有限公司 A kind of VPD metal recovery liquid and its compound method
CN107389663A (en) * 2017-06-30 2017-11-24 天津中环领先材料技术有限公司 A kind of method for detecting metal ion content in silicon chip surface oxide-film

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CN102980938A (en) * 2012-12-03 2013-03-20 天津中环领先材料技术有限公司 Method for testing metal ions on surface of wafer of solar battery
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Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN112683988A (en) * 2020-12-28 2021-04-20 上海新昇半导体科技有限公司 Method for detecting metal impurities in wafer
CN113130366A (en) * 2021-03-17 2021-07-16 江苏鲁汶仪器有限公司 Nozzle for wafer scanning and system and application thereof
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CN112713103B (en) * 2021-03-29 2021-06-25 西安奕斯伟硅片技术有限公司 Method for measuring metal content in silicon wafer
WO2023284205A1 (en) * 2021-07-16 2023-01-19 江苏鲁汶仪器有限公司 Online sampler and contamination analysis system
CN114459946A (en) * 2022-01-29 2022-05-10 西安奕斯伟材料科技有限公司 Method and equipment for testing metal content of silicon wafer
CN117168942A (en) * 2023-11-01 2023-12-05 山东有研艾斯半导体材料有限公司 Sampling method for detecting metal on surface of silicon wafer

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