CN110186994A - The processing analysis method and processing unit of heavy metal in a kind of silicon wafer - Google Patents

The processing analysis method and processing unit of heavy metal in a kind of silicon wafer Download PDF

Info

Publication number
CN110186994A
CN110186994A CN201910477207.0A CN201910477207A CN110186994A CN 110186994 A CN110186994 A CN 110186994A CN 201910477207 A CN201910477207 A CN 201910477207A CN 110186994 A CN110186994 A CN 110186994A
Authority
CN
China
Prior art keywords
silicon wafer
sample
chamber
container
hydrofluoric acid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910477207.0A
Other languages
Chinese (zh)
Inventor
宮尾秀一
张婉婉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian Eswin Material Technology Co Ltd
Original Assignee
Xian Eswin Silicon Wafer Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xian Eswin Silicon Wafer Technology Co Ltd filed Critical Xian Eswin Silicon Wafer Technology Co Ltd
Priority to CN201910477207.0A priority Critical patent/CN110186994A/en
Publication of CN110186994A publication Critical patent/CN110186994A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2873Cutting or cleaving

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Immunology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The present invention provides the processing analysis method and processing unit of heavy metal in a kind of silicon wafer, processing analysis method the following steps are included: cut on crystal orientation to silicon wafer to be processed, obtain include detection zone sample silicon wafer;The surface of sample silicon wafer is cleaned;Sample silicon wafer after cleaning is placed in the mixed vapour of nitric acid and hydrofluoric acid and is dissolved, sample silicon wafer treatment fluid is obtained.In processing analysis method of the invention, silicon wafer to be processed is cut on crystal orientation, obtain include detection zone sample silicon wafer, the surface of sample silicon wafer is cleaned, sample silicon wafer after cleaning is placed in the mixed vapour of nitric acid and hydrofluoric acid and is dissolved, obtain sample silicon wafer treatment fluid, the pollution of silicon wafer can be reduced by the above method, convenient for improving the accuracy of testing result when the analysis of subsequent silicon wafer, the dosage for reducing nitric acid and hydrofluoric acid, does not need the nitric acid and hydrofluoric acid of high-purity, reduces cost, Simplified analysis operating process, it is high-efficient.

Description

The processing analysis method and processing unit of heavy metal in a kind of silicon wafer
Technical field
The present invention relates to silicon chip technology field, in particular to the processing analysis method of heavy metal and processing dress in a kind of silicon wafer It sets.
Background technique
In the manufacturing process of silicon wafer, when being cut into silicon wafer from silicon ingot, blade or scroll saw are touched, heavy metal can be to silicon Diffusion inside piece.Heavy metal pollution most serious in polishing, due to two sides and the lapping liquid of silicon wafer, grinding pad long-time contact, Pressurization and grinding, are easy pollution by the impurity element from these materials, later can be to spreading inside silicon wafer.In reality, Aiming at the problem that impurity element in lapping liquid, by adding chelating agent in lapping liquid, chelating agent can be formed with heavy metal Chelate achievees the effect that capture heavy metal;Also not absolutely not metal impurities in grinding pad, in most cases, grinding pad It will use high molecular polymer, and most polymer will use metal as additive, metallic addition can also make silicon wafer At pollution.For the silicon wafer that inside is polluted by impurity element, in device fabrication behind, it can be taken the photograph several hundred to thousands of Heat treatment is repeated at a temperature of family name's degree, impurity element can spread repeatedly, move at this time, in made fine circuits easily The problems such as causing poor flow, short circuit, proof voltage decline.Therefore, the analysis detection of heavy metal is particularly important in silicon wafer.
When to silicon chip surface analysis, the mixed aqueous solution of hydrofluoric acid and nitric acid need to be dripped on silicon chip surface, be contacted and molten Solution corrodes entire silicon chip surface, then again recycles corrosive liquid, then analyzed by instruments such as ICP, analysis method detection Result error is big, and accuracy is low.About the analysis method of impurity in wafer bulk, pass through the metal analysis method for silicon chip surface Extension, successively silicon chip surface can be analyzed from longitudinal direction, but die size is increasing, is such as in diameter The silicon wafer of 300mm, it is extremely difficult that entire silicon chip surface equably carries out to depth profile, can generate because of position difference biggish Deviation.The thickness of silicon wafer is usually 780-800 μm, in order to dissolve this all areas, not only needs a large amount of hydrofluoric acid, nitre Acid, it is also necessary to which long time at least needs more than for three days on end, and efficiency is excessively poor, impracticable.In addition, if pretreatment time Longer, then environmental pollution and a possibility that wafer contamination, increase accordingly, can not Correct Analysis and assessment silicon wafer.It is carried out to silicon wafer The reagent that quite large-scale equipment and high-purity are needed when processing, cause it is at high cost, even if using these equipment and high-purity Reagent accurate value may not also can be obtained, actually it sometimes appear that a few % to 10% different degrees of exceptional value, it is difficult to really The accuracy and repeatability of detected value are protected, analysis operating process is continuously many and diverse, is unfavorable for the analysis detection of heavy metal in silicon wafer.
Summary of the invention
In view of this, the present invention provides the processing analysis method and processing unit of heavy metal in a kind of silicon wafer, to solve Vulnerable to pollution in silicon wafer treatment process, silicon wafer testing result accuracy is low, and the dosage of nitric acid and hydrofluoric acid is big, at high cost, efficiency Low problem.
In order to solve the above technical problems, the invention adopts the following technical scheme:
According to a first aspect of the present invention in the silicon wafer of embodiment heavy metal processing analysis method, comprising the following steps:
Silicon wafer to be processed is cut on crystal orientation, obtain include detection zone sample silicon wafer;
The surface of the sample silicon wafer is cleaned;
The sample silicon wafer after cleaning is placed in the mixed vapour of nitric acid and hydrofluoric acid and is dissolved, sample silicon is obtained Piece treatment fluid.
Further, the surface of the sample silicon wafer is cleaned, comprising:
The sample silicon wafer is placed in the mixed vapour of nitric acid and hydrofluoric acid, the surface of the sample silicon wafer is carried out clearly It washes.
Further, further comprising the steps of:
Hydrofluoric acid solution and evaporation drying are added into the sample silicon wafer treatment fluid, obtains the first processing sample;
The first processing sample is added in aqueous solution of nitric acid and obtains measurement solution;
Detect the heavy metal in the measurement solution.
The processing unit of the silicon wafer of embodiment according to a second aspect of the present invention, comprising:
Container, define in the container for accommodate include nitric acid solution and hydrofluoric acid solution mixed solution first Chamber and the second chamber being connected to the first chamber;
Heating mechanism, for heating the mixed solution in the first chamber, so that the mixed solution evaporates shape The second chamber is able to enter at the mixed vapour of nitric acid and hydrofluoric acid and the mixed vapour;
Sample box, the sample box are placed in the second chamber for containing sample silicon wafer, the mixed vapour energy Enough enter in the sample box so that the sample silicon wafer dissolves in the mixed vapour.
Further, the container is the metal material or ceramic material container that outside is coated with polytetrafluoroethylene (PTFE), described Heating mechanism includes mantle heater, and the mantle heater is set in the outside of the container.
Further, the container is column, and the first chamber is located at the bottom of the container, the second chamber position In the top of the container, columnar gas-guide tube, one end of the gas-guide tube and the first chamber are equipped in the container Open communication, the other end of the gas-guide tube protrude into the second chamber and are connected to the second chamber, the gas-guide tube The axis collinear of axis and the container.
Further, be respectively equipped with the air inlet and air outlet being connected to the second chamber on the container, it is described into Port and axisymmetrical of the gas outlet about the container, the neighbouring air inlet and the outlet in the second chamber The position of mouth is respectively equipped with the porous plate for having through-hole, axisymmetrical of two porous plates about the container, institute The quantity for stating sample box is multiple and is respectively placed on the corresponding porous plate.
Further, the processing unit further include:
Two thermometers, two thermometers are all set in the second chamber, one of them described thermometer position In the top of the gas-guide tube, another described thermometer is located at the top of the porous plate of the neighbouring gas outlet.
Further, the processing unit further include:
Inert gas feeding mechanism, the inert gas feeding mechanism are connected to the air inlet, with to second chamber Inert gas is passed through in room.
Further, connecting tube is equipped between the inert gas feeding mechanism and the air inlet to be connected to the inertia Gas supply device and the air inlet are respectively equipped with flowmeter and filter in the connecting tube.
The advantageous effects of the above technical solutions of the present invention are as follows:
The processing analysis method of heavy metal, cuts silicon wafer to be processed on crystal orientation in silicon wafer according to the present invention Cut, obtain include detection zone sample silicon wafer, the surface of sample silicon wafer is cleaned, the sample silicon wafer after cleaning is placed in It is dissolved in the mixed vapour of nitric acid and hydrofluoric acid, obtains sample silicon wafer treatment fluid, silicon wafer can be reduced by the above method Pollution, convenient for subsequent silicon wafer analysis when improve testing result accuracy, reduce nitric acid and hydrofluoric acid dosage, do not need height The nitric acid and hydrofluoric acid of purity, reduce cost, and Simplified analysis operating process is high-efficient.
Detailed description of the invention
Fig. 1 is the flow diagram of the processing analysis method of heavy metal in the silicon wafer of the embodiment of the present invention;
Fig. 2 is the structural schematic diagram of the processing unit of the embodiment of the present invention;
Fig. 3 is the partial structural diagram of the processing unit of the embodiment of the present invention.
Appended drawing reference
Container 10;First chamber 11;Second chamber 12;Gas-guide tube 13;
Air inlet 14;Gas outlet 15;Porous plate 16;Thermometer 17;
Heating mechanism 20;
Sample box 30;
Inert gas feeding mechanism 40;Flowmeter 41;Filter 42.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention Attached drawing, the technical solution of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is this hair Bright a part of the embodiment, instead of all the embodiments.Based on described the embodiment of the present invention, ordinary skill Personnel's every other embodiment obtained, shall fall within the protection scope of the present invention.
The processing analysis method of heavy metal in silicon wafer according to an embodiment of the present invention is detailed below.
As shown in Figure 1, in silicon wafer according to an embodiment of the present invention heavy metal processing analysis method, comprising the following steps: Silicon wafer to be processed is cut on crystal orientation, obtain include detection zone sample silicon wafer;To the surface of sample silicon wafer It is cleaned;Sample silicon wafer after cleaning is placed in the mixed vapour of nitric acid and hydrofluoric acid and is dissolved, sample silicon wafer is obtained Treatment fluid.
That is, the size due to silicon wafer is larger, it can be cut into and the region detected is needed to be examined after treatment Survey, silicon wafer to be processed can be cut on crystal orientation, obtain include detection zone sample silicon wafer, sample silicon wafer weight Amount can be 0.30-0.35g, and the surface diameter of sample silicon wafer is 5mm or so;Then the surface of sample silicon wafer is cleaned, clearly The pollution impurity of silicon chip surface is washed away, one layer of silicon on the surface of silicon wafer can be dissolved, then the solution of dissolution is gone, is kept away The pollution for exempting from the impurity on silicon chip surface, the silicon wafer weight after cleaning can be 0.15-0.2g, use polytetrafluoroethyl-ne in the operation The tweezers of alkene carry out, and avoid introducing metal impurities;Then, the sample silicon wafer after cleaning is placed in the mixing of nitric acid and hydrofluoric acid It is dissolved in steam, obtains sample silicon wafer treatment fluid, do not need the nitric acid and hydrofluoric acid of high-purity, reduce nitric acid and hydrofluoric acid Dosage, the pollution of silicon wafer can be reduced by the above method, convenient for subsequent silicon wafer analysis when improve testing result accuracy, Testing result repeatability is stable and good, will not generate exceptional value, reduce cost, Simplified analysis operating process is high-efficient.Separately Outside, prepared using silicon wafer device requirement be ultramicron concentration rank, in order to avoid introduce impurity, can in toilet into Row, it preferably can be 10 or 1 grades that the minimum cleanliness of toilet, which can be 100 grades,.
In some embodiments of the invention, the surface of sample silicon wafer is carried out cleaning includes: that sample silicon wafer is placed in nitre The surface of sample silicon wafer is cleaned in the mixed vapour of acid and hydrofluoric acid, by the mixed vapour of nitric acid and hydrofluoric acid to sample Product silicon wafer is cleaned, and is enabled to one layer of silicon on the surface of sample silicon wafer to dissolve, is avoided surface impurity to sample silicon wafer rear Influence in continuous detection, does not need the nitric acid and hydrofluoric acid of high-purity, reduces the dosage of nitric acid and hydrofluoric acid, at low cost.
It is further comprising the steps of in other embodiments of the invention: hydrofluoric acid is added into sample silicon wafer treatment fluid Solution and evaporation drying, obtain the first processing sample;First processing sample is added in aqueous solution of nitric acid and obtains measurement solution;Inspection Heavy metal in measurement solution.It that is to say, hydrofluoric acid solution is added into obtained sample silicon wafer treatment fluid, and evaporate dry It is dry, sample silicon wafer treatment fluid can be placed in sample box, the solvent of sample box can reasonably select, for example can be 2ml, to Hydrofluoric acid solution is added in sample box, hydrofluoric acid solution can be 5wt% hydrofluoric acid solution, can be on hot plate in 200 DEG C Under be evaporated to drying, obtain the first processing sample;Hereafter, the first processing sample can be added in aqueous solution of nitric acid and is measured Solution, for example, aqueous solution of nitric acid can be 1ml 0.5wt% aqueous solution of nitric acid, obtain measurement solution after, by detecting instrument into Heavy metal in row detection measurement solution, detecting instrument can be ICP-MS (inductivity coupled plasma mass spectrometry), in ICP-MS Before detection, normal concentration solution can be prepared for every kind of element in advance, and prepare calibration curve.
Hydrofluoric acid solution is the hydrofluoric acid solution of 38wt%, and nitric acid solution is the nitric acid solution of 55wt%, which needs It is ultrapure, ICP-MS can be introduced directly into.In actual analytic process, for medical fluid used in ventilation distillate, it can be used ICP-MS measures two kinds of blank solutions, the first is the hydrofluoric acid and nitre of the TAMAPURE-AA-100 of the chemistry systems of rubbing of high-purity more Acid, passes through above two hydrofluoric acid and nitre when being the superfine hydrofluoric acid and nitric acid of electron level, using method of the invention second Measurement result such as the following table 1 when acid is measured:
Table 1 is the measurement result of different hydrofluoric acid and nitric acid
Wherein, the unit of the measured value in table 1 is pptw, is the concentration of the Unit Weight of silicon sample, it can be seen from this result that, It ventilates the not big difference of grade of hydrofluoric acid used in distillate, nitric acid, the grade of special grade chemical can be met the requirements.
The embodiment of the present invention also provides a kind of processing unit of silicon wafer, and as shown in Figures 2 and 3, processing unit includes container 10, heating mechanism 20 and sample box 30.
Specifically, defined in container 10 for accommodate include nitric acid solution and hydrofluoric acid solution mixed solution the One chamber 11 and the second chamber 12 being connected to first chamber 11, the mixing that heating mechanism 20 is used to heat in first chamber 11 are molten Liquid, so that mixed solution evaporates the mixed vapour to form nitric acid and hydrofluoric acid and mixed vapour is able to enter second chamber 12, sample Product box 30 is placed in second chamber 12 so that for containing sample silicon wafer, mixed vapour is able to enter in sample box 30 so that sample silicon Piece dissolves in mixed vapour.
That is, processing unit is mainly made of container 10, heating mechanism 20 and sample box 30, wherein in container 10 First chamber 11 and second chamber 12 can be defined, first chamber 11 is connected to second chamber 12, and first chamber 11 can be used In accommodating mixed solution, mixed solution includes nitric acid solution and hydrofluoric acid solution.Heating mechanism 20 can be used for heating the first chamber Mixed solution in room 11, so that mixed solution evaporates the mixed vapour to form nitric acid and hydrofluoric acid, and mixed vapour can be into Enter in second chamber 12, sample box 30 can be placed in second chamber 12, and sample box 30 can be used for containing sample silicon wafer, sample The volume of box 30 can reasonably select, for example can be 2ml, and sample box 30 can be into for one or more, mixed vapour Enter in sample box 30 so that sample silicon wafer dissolves in mixed vapour.When the surface to sample silicon wafer is cleaned, can incite somebody to action Sample silicon wafer is placed in sample box 30, by mixed vapour sample dissolution silicon wafer, is then gone dissolved solution, then will be clear Sample silicon wafer after washing, which is placed in the mixed vapour of nitric acid and hydrofluoric acid, to be dissolved, and sample silicon wafer treatment fluid is obtained, by upper Stating device can be realized the cleaning and dissolution of sample silicon wafer, not need the nitric acid and hydrofluoric acid of high-purity, reduce nitric acid and hydrogen fluorine The dosage of acid, it is easy to operate, the pollution of silicon wafer can be reduced, convenient for improving the accuracy of testing result when the analysis of subsequent silicon wafer, Cost is reduced, it is high-efficient.
In some embodiments of the invention, container 10 can be coated with the metal material or pottery of polytetrafluoroethylene (PTFE) for outside Porcelain material container 10, for example can be the stainless steel pressure vessel for being coated with polytetrafluoroethylene (PTFE), heating mechanism 20 may include cover Shape heater, mantle heater can be set in the outside of container 10, convenient for carrying out heating and thermal insulation to container 10, so that container 10 It is middle to keep stable temperature, prevent steam from condensing.
In other embodiments of the invention, container 10 can be column, and first chamber 11 is located at the bottom of container 10, Second chamber 12 is located at the top of container 10, can be equipped with columnar gas-guide tube 13 in container 10, one end of gas-guide tube 13 and the The open communication of one chamber 11, the other end of gas-guide tube 13 are protruded into second chamber 12 and are connected to second chamber 12, convenient for the Steam in one chamber 11 enters in second chamber 12 so that steam can sample silicon wafer preferably in sample dissolution box 30, The axis collinear of the axis of gas-guide tube 13 and container 10 enables the steam in first chamber 11 uniformly and stably to enter the In two chambers 12, the sample silicon wafer in the sample box 30 in second chamber 12 is uniformly and stably contacted with steam, just In the dissolution of silicon wafer, silicon wafer is enabled equably to keep rate of dissolution constant.
According to some embodiments of the present invention, the air inlet 14 being connected to second chamber 12 can be respectively equipped on container 10 With gas outlet 15, air inlet 14 and gas outlet 15 can be about the axisymmetricals of container 10, can be symmetrical about gas-guide tube 13, the The position of neighbouring air inlet 14 and gas outlet 15 can be respectively equipped with the porous plate 16 for having through-hole in two chambers 12, namely It is that a porous plate 16 is arranged in the position of neighbouring air inlet 14 in second chamber 12, the neighbouring gas outlet in second chamber 12 A porous plate 16 is arranged in 15 position, and two porous plates 16 can be about the axisymmetrical of container 10, the quantity of sample box 30 It is multiple, for example can is six, and sample box 30 can be respectively placed on corresponding porous plate 16, and sample box 30 can be about The axisymmetrical of container 10 is distributed, so that the steam in first chamber 11 can uniformly and stably enter different sample boxes 30 In.In order to quickly dissolve silicon, need to be heated at high temperature, so that the solution in first chamber 11 evaporates, actual temp can be reasonable Selection, for example can choose at 100 DEG C or more, heating is main at such a temperature occurs following reaction: Si+2HNO3+6HF→ H2SiF6+NO↑+NO2↑+3H2O, Δ H=-85.2kcal/mol (exothermic reaction), the gas (NO that the dissolution reaction of silicon generates2、 NO it) is not easy to discharge, therefore the pressure in container rises, it can be convenient for generation by setting air inlet 14 and gas outlet 15 Gas outflow, is conducive to the progress of dissolution reaction, convenient for accelerating dissolution.
Other embodiments according to the present invention, processing unit can also include two thermometers 17, two thermometers 17 It is all set in second chamber 12, one of thermometer 17 can be located at the top of gas-guide tube 13, another thermometer 17 can To be located at the top of the porous plate 16 of neighbouring gas outlet 15, the temperature in second chamber 12 can be monitored by two thermometers 17 Degree.
In some embodiments of the invention, processing unit can also include inert gas feeding mechanism 40, inert gas Feeding mechanism 40 can be connected to air inlet 14, can band by inert gas to be passed through inert gas into second chamber 12 Walk silicon materials, for example, in inert gas feeding mechanism 40 can be equipped with nitrogen, by inert gas feeding mechanism 40 can from into Port 14 is passed through nitrogen into second chamber 12.
In other embodiments of the invention, connection can be equipped between inert gas feeding mechanism 40 and air inlet 14 Pipe, can be connected to inert gas feeding mechanism 40 and air inlet 14 by connecting tube, 41 He of flowmeter is respectively equipped in connecting tube Filter 42 can monitor the flow for the inert gas being passed through in second chamber 12 by flowmeter 41, can by filter 42 It is passed through the inert gas in second chamber 12 with filtration, purification, avoids bringing impurity into.In actual application, two thermometers 17 can measure the temperature of the different parts in second chamber 12, and adjustable inert gas is passed through the temperature one for making the two Cause, the dissolution of silicon materials can be adjusted by steam and inert gas, then by evaporation make silicon materials with wherein contain it is miscellaneous Prime element separation, convenient for the detection of impurity element.
In application process, 30 volume of sample box can be 2ml, be added 300ml volume ratio 1:1's in first chamber 11 The nitric acid solution of 50wt% hydrofluoric acid solution and 70wt%, the mixed solution heated in first chamber 11 generate steam, first carry out The surface washing of silicon wafer, at this point, solution need not boil, as long as steam can be generated.About the ventilatory capacity of inert gas, in order to Make two thermometer equalities of temperature, ventilatory capacity can be 50ml/min, and the temperature in first chamber 11 can be 73-75 DEG C, at this After carrying out the distillation of ventilation in 2 hours under part, distillation is temporarily ceased, confirms the etching state of silicon wafer and the residual component of solution and silicon The weight of piece;It is again started up processing unit and carries out distillation generation steam, can carry out steaming for 2 hours again to be completely dissolved silicon wafer It evaporates, then, by processing unit natural cooling, confirms silicon wafer and be completely dissolved, solution has remained 100ml or so.
Different types of silicon wafer can be measured by the above method and device, specific measurement result such as the following table 2, Table 3, table 4 and table 5.
Table 2 is the testing result of the center and peripheral of N-type non-impurity-doped 300mm silicon wafer
Table 3 is the testing result of the center and peripheral of 1 Ω-cm 300mm silicon wafer of N-type
Table 4 is the testing result of the center and peripheral of p-type non-impurity-doped 300mm silicon wafer
Table 5 is the testing result of the center and peripheral of 0.001 Ω-cm 300mm silicon wafer of p-type
It is shown by the measurement result in above-mentioned table, the comparison of four kinds of different silicon wafers (N-type, p-type and doped level) shows P Impurity in type doped silicon wafer is very high, and reason is that the silicon wafer has lesser polished amount, i.e., polishing removal per unit time Measure it is less, about -10% to -15% because it is harder than other silicon wafers, it is desirable that polishing time is long, thus impurity pollution it is more.This Outside, for all types of chips, impurity is lower and higher in edge at center, may be in the CZ except polishing and processing It is introduced in process.As described above, can track and verify and is inside from surface by carrying out impurity and volumetric analysis in silicon wafer The element of portion's diffusion, and process modification can be carried out, to avoid the impurity contact in polishing process.On the other hand, in order to test It demonstrate,proves whether the pre-treating method accurately works, impurity element is made an addition in silicon chip sample, measure its rate of recovery, it is specific real In applying method, the standard solution for corresponding to 20pptw concentration is added in sample silicon wafer, which completes above-mentioned surface Cleaning and dissolution, measure impurity element concentration and the rate of recovery, the silicon wafer sample for measurement is 1 Ω-cm 300mm silicon wafer of N-type Central part, testing result such as following table 6.
Table 6 is the testing result for adding the silicon wafer after impurity element
The rate of recovery is good for all elements, demonstrate this method be accurately, according to this method, by silicon dissolution, It removes, gasification, stops contained impurity element directly and be deposited in container, the impurity member for including by principal component silicon and ultramicron Element separation, separation completeness are high.Method in through the embodiment of the present invention can also contribute to understanding in silicon wafer manufacturing process Actual conditions of the metal to diffusion, pollution inside silicon wafer.
Unless otherwise defined, technical term or scientific term used in the present invention are should be in fields of the present invention The ordinary meaning that personage with general technical ability is understood." first ", " second " used in the present invention and similar word It is not offered as any sequence, quantity or importance, and is used only to distinguish different component parts." connection " or " connected " It is not limited to physics or mechanical connection etc. similar word, but may include electrical connection, either directly Or it is indirect."upper", "lower", "left", "right" etc. are only used for indicating relative positional relationship, when the absolute position for being described object After setting change, then the relative positional relationship also correspondingly changes.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications It should be regarded as protection scope of the present invention.

Claims (10)

1. the processing analysis method of heavy metal in a kind of silicon wafer, which comprises the following steps:
Silicon wafer to be processed is cut on crystal orientation, obtain include detection zone sample silicon wafer;
The surface of the sample silicon wafer is cleaned;
The sample silicon wafer after cleaning is placed in the mixed vapour of nitric acid and hydrofluoric acid and is dissolved, is obtained at sample silicon wafer Manage liquid.
2. processing analysis method according to claim 1, which is characterized in that carry out the surface of the sample silicon wafer clear It washes, comprising:
The sample silicon wafer is placed in the mixed vapour of nitric acid and hydrofluoric acid, the surface of the sample silicon wafer is cleaned.
3. processing analysis method according to claim 1, which is characterized in that further comprising the steps of:
Hydrofluoric acid solution and evaporation drying are added into the sample silicon wafer treatment fluid, obtains the first processing sample;
The first processing sample is added in aqueous solution of nitric acid and obtains measurement solution;
Detect the heavy metal in the measurement solution.
4. a kind of processing unit of silicon wafer characterized by comprising
Container, define in the container for accommodate include nitric acid solution and hydrofluoric acid solution mixed solution first chamber The second chamber being connected to with the first chamber;
Heating mechanism, for heating the mixed solution in the first chamber, so that the mixed solution evaporates to form nitre Acid and hydrofluoric acid mixed vapour and the mixed vapour be able to enter the second chamber;
Sample box, the sample box are placed in the second chamber with for containing sample silicon wafer, and the mixed vapour can be into Enter in the sample box so that the sample silicon wafer dissolves in the mixed vapour.
5. processing unit according to claim 4, which is characterized in that the container is that outside is coated with polytetrafluoroethylene (PTFE) Metal material or ceramic material container, the heating mechanism include mantle heater, and the mantle heater is set in the appearance The outside of device.
6. processing unit according to claim 4, which is characterized in that the container is column, and the first chamber is located at The bottom of the container, the second chamber are located at the top of the container, and columnar gas-guide tube is equipped in the container, described The open communication of one end of gas-guide tube and the first chamber, the other end of the gas-guide tube protrude into the second chamber and with institute State second chamber connection, the axis collinear of the axis of the gas-guide tube and the container.
7. processing unit according to claim 6, which is characterized in that be respectively equipped on the container and the second chamber The air inlet and air outlet of connection, the air inlet and axisymmetrical of the gas outlet about the container, second chamber The position of the neighbouring air inlet and the gas outlet is respectively equipped with the porous plate for having through-hole in room, and two described porous Axisymmetrical of the plate about the container, the quantity of the sample box are multiple and are respectively placed on the corresponding porous plate.
8. processing unit according to claim 7, which is characterized in that further include:
Two thermometers, two thermometers are all set in the second chamber, one of them described thermometer is located at institute The top of gas-guide tube is stated, another described thermometer is located at the top of the porous plate of the neighbouring gas outlet.
9. processing unit according to claim 7, which is characterized in that further include:
Inert gas feeding mechanism, the inert gas feeding mechanism is connected to the air inlet, into the second chamber It is passed through inert gas.
10. processing unit according to claim 9, which is characterized in that the inert gas feeding mechanism and the air inlet It is equipped with connecting tube between mouthful to be connected to the inert gas feeding mechanism and the air inlet, is respectively equipped with stream in the connecting tube Meter and filter.
CN201910477207.0A 2019-06-03 2019-06-03 The processing analysis method and processing unit of heavy metal in a kind of silicon wafer Pending CN110186994A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910477207.0A CN110186994A (en) 2019-06-03 2019-06-03 The processing analysis method and processing unit of heavy metal in a kind of silicon wafer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910477207.0A CN110186994A (en) 2019-06-03 2019-06-03 The processing analysis method and processing unit of heavy metal in a kind of silicon wafer

Publications (1)

Publication Number Publication Date
CN110186994A true CN110186994A (en) 2019-08-30

Family

ID=67719964

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910477207.0A Pending CN110186994A (en) 2019-06-03 2019-06-03 The processing analysis method and processing unit of heavy metal in a kind of silicon wafer

Country Status (1)

Country Link
CN (1) CN110186994A (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111344852A (en) * 2020-02-10 2020-06-26 长江存储科技有限责任公司 Metal contamination testing device and method
CN111624460A (en) * 2020-06-28 2020-09-04 西安奕斯伟硅片技术有限公司 Method for detecting defect distribution area of monocrystalline silicon
CN112539982A (en) * 2020-12-03 2021-03-23 西安奕斯伟硅片技术有限公司 Silicon wafer sample and manufacturing method thereof
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
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
CN117191932A (en) * 2023-11-06 2023-12-08 山东有研艾斯半导体材料有限公司 Method and system for testing metal recovery rate of silicon wafer surface
WO2024001016A1 (en) * 2022-06-29 2024-01-04 江苏鲁汶仪器有限公司 Enrichment method and analysis method for precious metal elements on surface of wafer

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07333121A (en) * 1994-06-10 1995-12-22 Toshiba Ceramics Co Ltd Treatment method for highly precise analysis of impurity in siliceous analysis sample and apparatus therefor
CN1993293A (en) * 2004-08-06 2007-07-04 旭化成化学株式会社 Method for purifying aqueous alkaline solution
CN101219564A (en) * 2007-12-27 2008-07-16 北京交通大学 Silicon slice cutting method
CN104568535A (en) * 2013-10-29 2015-04-29 中芯国际集成电路制造(上海)有限公司 VPD sample collection method
CN107123608A (en) * 2017-06-19 2017-09-01 浙江晶科能源有限公司 A kind of solar cell processing procedure metal ion pollution detection method and device
CN109680340A (en) * 2019-02-27 2019-04-26 南京航空航天大学 A kind of fluff making device of Buddha's warrior attendant wire cutting polysilicon chip
CN109701947A (en) * 2019-01-04 2019-05-03 内蒙古鄂尔多斯电力冶金集团股份有限公司 A kind of cleaning device and cleaning method of polycrystalline silicon material
CN109830435A (en) * 2019-02-01 2019-05-31 天津中环领先材料技术有限公司 A kind of device and method removing silicon chip surface silicon dioxide film

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07333121A (en) * 1994-06-10 1995-12-22 Toshiba Ceramics Co Ltd Treatment method for highly precise analysis of impurity in siliceous analysis sample and apparatus therefor
CN1993293A (en) * 2004-08-06 2007-07-04 旭化成化学株式会社 Method for purifying aqueous alkaline solution
CN101219564A (en) * 2007-12-27 2008-07-16 北京交通大学 Silicon slice cutting method
CN104568535A (en) * 2013-10-29 2015-04-29 中芯国际集成电路制造(上海)有限公司 VPD sample collection method
CN107123608A (en) * 2017-06-19 2017-09-01 浙江晶科能源有限公司 A kind of solar cell processing procedure metal ion pollution detection method and device
CN109701947A (en) * 2019-01-04 2019-05-03 内蒙古鄂尔多斯电力冶金集团股份有限公司 A kind of cleaning device and cleaning method of polycrystalline silicon material
CN109830435A (en) * 2019-02-01 2019-05-31 天津中环领先材料技术有限公司 A kind of device and method removing silicon chip surface silicon dioxide film
CN109680340A (en) * 2019-02-27 2019-04-26 南京航空航天大学 A kind of fluff making device of Buddha's warrior attendant wire cutting polysilicon chip

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111344852B (en) * 2020-02-10 2021-08-31 长江存储科技有限责任公司 Metal contamination testing device and method
CN111344852A (en) * 2020-02-10 2020-06-26 长江存储科技有限责任公司 Metal contamination testing device and method
US11302524B2 (en) 2020-02-10 2022-04-12 Yangtze Memory Technologies Co., Ltd. Metal contamination test apparatus and method
WO2021159225A1 (en) * 2020-02-10 2021-08-19 Yangtze Memory Technologies Co., Ltd. Metal contamination test apparatus and method
CN111624460A (en) * 2020-06-28 2020-09-04 西安奕斯伟硅片技术有限公司 Method for detecting defect distribution area of monocrystalline silicon
CN111624460B (en) * 2020-06-28 2022-10-21 西安奕斯伟材料科技有限公司 Method for detecting defect distribution area of monocrystalline silicon
CN112539982B (en) * 2020-12-03 2023-11-03 西安奕斯伟材料科技股份有限公司 Manufacturing method of silicon wafer sample and silicon wafer sample
CN112539982A (en) * 2020-12-03 2021-03-23 西安奕斯伟硅片技术有限公司 Silicon wafer sample and manufacturing method thereof
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
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
WO2024001016A1 (en) * 2022-06-29 2024-01-04 江苏鲁汶仪器有限公司 Enrichment method and analysis method for precious metal elements on surface of 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
CN117191932A (en) * 2023-11-06 2023-12-08 山东有研艾斯半导体材料有限公司 Method and system for testing metal recovery rate of silicon wafer surface

Similar Documents

Publication Publication Date Title
CN110186994A (en) The processing analysis method and processing unit of heavy metal in a kind of silicon wafer
EP0597792A2 (en) Device and method for accurate etching and removal of thin film
KR19990029782A (en) Semiconductor wafer temperature measurement and control device using gas temperature measurement and its method
JPH05326480A (en) Surface treatment apparatus for semiconductor substrate and control method therefor
US20050208674A1 (en) Method for analyzing impurities
CN100365174C (en) Process for treating a semiconductor wafer with a gaseous medium, and semiconductor wafer treated by this process
CN101769848B (en) Method for detecting etching fluid filter
EP0137409A2 (en) Resolution device for semiconductor thin films
KR101239394B1 (en) Method of estimating water quality, estimation apparatus and preparation system of ultra-pure water using the same
US11728188B2 (en) Semiconductor manufacturing device
JP2013041923A (en) Device for measuring silicon concentration in phosphate solution, and measuring method therefor
WO2003036706A1 (en) Method and apparatus for etching silicon wafer and method for analysis of impurities
JP5459053B2 (en) Impurity evaluation method of silicon single crystal
JP5120789B2 (en) Method for evaluating contamination of semiconductor manufacturing equipment
TW202225687A (en) Method for measuring superficial metal content of a wafer
JP2008182201A (en) Silicon etching method
JP2001194362A (en) Method and apparatus for extracting impurities in semi conductor substrate
JP2001153854A5 (en)
CN109580320A (en) The pre-treating method and device that trace impurity is analyzed in electron level ethyl orthosilicate
JP3286215B2 (en) Surface analysis method for silicon wafer
JP2001242052A (en) Method for analyzing impurity in semiconductor substrate or chemicals
JP4000027B2 (en) Semiconductor sample impurity analysis method and semiconductor sample impurity concentration apparatus
KR101730354B1 (en) Purification apparatus of hydrofluoric acid
JP2019200061A (en) Measuring apparatus and measuring method of dissolved gas concentration
CN117080050A (en) Thermal oxidation reaction device

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right
TA01 Transfer of patent application right

Effective date of registration: 20211009

Address after: 710000 room 1-3-029, No. 1888, Xifeng South Road, high tech Zone, Xi'an, Shaanxi Province

Applicant after: Xi'an yisiwei Material Technology Co.,Ltd.

Applicant after: XI'AN ESWIN SILICON WAFER TECHNOLOGY Co.,Ltd.

Address before: 710065 room 1323, block a, city gate, No. 1, Jinye Road, high tech Zone, Xi'an, Shaanxi Province

Applicant before: XI'AN ESWIN SILICON WAFER TECHNOLOGY Co.,Ltd.

RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190830