CN102097291B - Repair regeneration method of reference piece for heavy metal pollution for silicon wafer and regeneration solution - Google Patents
Repair regeneration method of reference piece for heavy metal pollution for silicon wafer and regeneration solution Download PDFInfo
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- CN102097291B CN102097291B CN2010105232632A CN201010523263A CN102097291B CN 102097291 B CN102097291 B CN 102097291B CN 2010105232632 A CN2010105232632 A CN 2010105232632A CN 201010523263 A CN201010523263 A CN 201010523263A CN 102097291 B CN102097291 B CN 102097291B
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Abstract
The invention relates to a repair and regeneration solution of a heavy metal polluted testing reference piece for a silicon wafer. The solution comprises a solution A, a solution D, a solution B and a solution C, wherein the solution A is 30wt% hydrogen peroxide; the solution D is a dissolved solution of aluminium potassium sulfate dodecahydrate in H2SO4; 0.15-0.21g of aluminium potassium sulfate dodecahydrate is dissolved in 100ml of H2SO4; the solution B is mixed liquor of fluorinated ammonia and hydrofluoric acid; 140-200ml of hydrofluoric acid is mixed in 1000ml of fluorinated ammonia; the solution C is aqueous solution of hydrofluoric acid; and 230-300ml of hydrofluoric acid is added to 1000ml of water. The invention also provides a relevant repair and regeneration method. The solution and the method have the following beneficial effects: the design is unique; the operation is simple and convenient; the effect is obvious; the problem of retreatment and reuse of the testing reference piece after pollution can be solved; normal testing use is fully satisfied; the testing and manufacturing costs of the enterprises can be greatly lowered; and the solution and the method are suitable for large-scale popularization and application.
Description
Technical field
The present invention relates to technical field of manufacturing semiconductors, be specifically related to test reference chip technology field, particularly a kind of reparative regeneration method and associated restoration actified solution of silicon chip heavy metal pollution test reference sheet.
Background technology
In semiconductor fabrication; The equipment of contact product and smelting tool very easily form product and pollute, and wherein staiing composition mainly is metal ions such as Fe, Cu; Silicon wafer to manufacture after the metallic pollution can have a strong impact on quality of oxide layer after becoming device, reduces the reliability and the rate of finished products of device.
SPV (surface photovoltaic method) is a kind of non-destructive advanced method of the silicon polished minority carrier lifetime of sheet scanning survey, diffusion length and metals content impurity entirely, utilizes this SPV method (adopting the SPV measurement mechanism) can measure the content of the silicon polished minority carrier life time of p type, diffusion length and iron tramp concentration.
SPV measurement mechanism measuring principle figure sees also illustrated in figures 1 and 2, and wherein 1 is electronics.Generally; Iron tramp in the P type silicon chip is to be combined into " FE-B " to 2 with dopant boron, and when SPV adopts the near infrared light radiation sample of stronger wavelength greater than 0.7UM, " FE-B " of P type silicon sample resolves into interstitial iron atom 3 to 2; Gap FE atom 3 is very effective minority carrier recombination centers; Its corresponding energy level is in Ev+0.4eV, and " FE-B " is in Ev+0.1eV to 2 corresponding energy levels, and its electron capture coefficient is merely 1/12 of interstitial iron atom 3.After heat or light had been encouraged, Fe-B was owing to catch the cause of separate electronic, and the life-span can reduce with diffusion is long.Calculate the concentration of Fe: NFe-B=1.05 * E16 * (1/Laft2-1/Lbef2) through twice minority diffusion length value before and after the contrast.
For accuracy and the reliability that guarantees measurement result, need carry out spot check and correction to testing apparatus SPV with the test reference sheet of known reference value, carry out the test of silicon chip after affirmation equipment is normal again.This test reference sheet is very easily polluted in test and use, and sensitivity, diffusion length can reduce, and not only influences precision of test result but also has influence on the normal mensuration use of equipment.
If the practice that the test reference sheet receives pollution, take at present is: 1. contaminated test reference sheet is scrapped processing.2. buy the test reference sheet again.3. entrust external agency to make the test reference sheet again.Exist deficiency to have: 1. procurement cycle is long.2. cost is very high.3. particularly domestic seldom have this test reference sheet to sell, very easily cause SPV equipment normally to use.
In order to solve the problems referred to above of existence; A kind of reparative regeneration method of silicon chip heavy metal pollution test reference sheet need be provided; The problem of processing and utilizing again that it can solve after the test reference sheet pollutes fully satisfies proper testing and uses, and can reduce the test and the manufacturing cost of enterprise greatly.
Summary of the invention
The objective of the invention is to have overcome above-mentioned shortcoming of the prior art, a kind of reparative regeneration method and associated restoration actified solution of silicon chip heavy metal pollution test reference sheet is provided, the reparative regeneration method design of this silicon chip heavy metal pollution test reference sheet is unique; Easy and simple to handle; Effect is remarkable, can solve the problem of processing and utilizing again after the test reference sheet pollutes, and fully satisfies proper testing and uses; And can reduce the test and the manufacturing cost of enterprise greatly, be suitable for large-scale promotion application.
To achieve these goals, in first aspect of the present invention, a kind of reparative regeneration solution of silicon chip heavy metal pollution test reference sheet is provided; Be characterized in; Comprise A solution and D solution, said A solution is the hydrogen peroxide of 30wt%, and said D solution is that Potassium aluminum sulfate dodecahydrate is at H
2SO
4In lysate, the said H of 100ml wherein
2SO
4In be dissolved with the said Potassium aluminum sulfate dodecahydrate of 0.15～0.21g.
In second aspect of the present invention; A kind of reparative regeneration solution of silicon chip heavy metal pollution test reference sheet is provided, has been characterized in, comprised B solution; Said B solution is the mixed liquor of ammonium fluoride and hydrofluoric acid, wherein is mixed with the said hydrofluoric acid of 140～200ml in the said ammonium fluoride of 1000ml.
In the third aspect of the invention, a kind of reparative regeneration solution of silicon chip heavy metal pollution test reference sheet is provided, be characterized in that comprise C solution, said C solution is the aqueous solution of hydrofluoric acid, wherein adding in the said water of 1000ml has the said hydrofluoric acid of 230～300ml.
In fourth aspect of the present invention, a kind of reparative regeneration method of silicon chip heavy metal pollution test reference sheet is provided, be characterized in, comprise the following steps:
A) A solution is placed reparative regeneration vessel in heating to 70～80 ℃; Add D solution; Put into said silicon chip heavy metal pollution test reference sheet then and handled 10～40 minutes, wherein said A solution is the hydrogen peroxide of 30wt%, and said D solution is that Potassium aluminum sulfate dodecahydrate is at H
2SO
4In lysate, the said H of 100ml wherein
2SO
4In be dissolved with the said Potassium aluminum sulfate dodecahydrate of 0.15～0.21g.
A) take out the said silicon chip heavy metal pollution test reference sheet of having handled, then with pure water rinsing and dry.
Need to prove that above-mentioned reparative regeneration method is suitable for handling N type reference plate.
Aspect the of the present invention the 5th, a kind of reparative regeneration method of silicon chip heavy metal pollution test reference sheet is provided, be characterized in, comprise the following steps:
A) B solution or C solution are placed said reparative regeneration container; Putting into said silicon chip heavy metal pollution test reference sheet handles below 40 minutes; Wherein said B solution is the mixed liquor of ammonium fluoride and hydrofluoric acid; Wherein be mixed with the said hydrofluoric acid of 140～200ml in the said ammonium fluoride of 1000ml, said C solution is the aqueous solution of hydrofluoric acid, and wherein adding in the said water of 1000ml has the said hydrofluoric acid of 230～300ml;
B) take out the said silicon chip heavy metal pollution test reference sheet of having handled, then with pure water rinsing and dry.
Need to prove that above-mentioned reparative regeneration method is suitable for handling P type reference plate.
Beneficial effect of the present invention is: through the reparative regeneration solution and the reparative regeneration method of silicon chip heavy metal pollution test reference sheet of the present invention; Can reparative regeneration silicon chip heavy metal pollution test reference sheet; Not only solved the problem of processing and utilizing again after the test reference sheet pollutes; Fully satisfy proper testing and use, and greatly reduce the test and the manufacturing cost of enterprise, be suitable for large-scale promotion application.
Description of drawings
Fig. 1 is a Fe-B bonding state sketch map generally.
Fig. 2 is SPV test Fe and a B released state sketch map down.
Embodiment
In order more to be expressly understood technology contents of the present invention, the special following examples of lifting specify.
N type reference plate handling process:
Embodiment one
Get a container, pour 100ml H into
2SO
4, accurately weighing 0.15g Potassium aluminum sulfate dodecahydrate is poured into wherein again, and stirring makes it to be dissolved as fully D solution, gets a reparative regeneration container again, pours the 10000mlA solution (H of 30wt% into
2O
2), be heated to 70～80 ℃, D solution is poured into, put into silicon chip heavy metal pollution test reference sheet and handled 10～40 minutes.Take out the silicon chip heavy metal pollution test reference sheet of having handled, pure water rinsing, drying are tested with SPV.
Embodiment two
Get a container, pour 100ml H into
2SO
4, accurately weighing 0.18g Potassium aluminum sulfate dodecahydrate is poured into wherein again, and stirring makes it to be dissolved as fully D solution, gets a reparative regeneration container again, pours the 10000mlA solution (H of 30wt% into
2O
2), be heated to 70～80 ℃, D solution is poured into, put into silicon chip heavy metal pollution test reference sheet and handled 10～40 minutes.Take out the silicon chip heavy metal pollution test reference sheet of having handled, pure water rinsing, drying are tested with SPV.
Embodiment three
Get a container, pour 100ml H into
2SO
4, accurately weighing 0.21g Potassium aluminum sulfate dodecahydrate is poured into wherein again, and stirring makes it to be dissolved as fully D solution, gets a reparative regeneration container again, pours the 10000mlA solution (H of 30wt% into
2O
2), be heated to 70～80 ℃, D solution is poured into, put into silicon chip heavy metal pollution test reference sheet and handled 10～40 minutes.Take out the silicon chip heavy metal pollution test reference sheet of having handled, pure water rinsing, drying are tested with SPV.
Test reference sheet in the foregoing description one to three is measured the result with the processing back and is gathered as follows before processing:
Embodiment four
Get a reparative regeneration container, pour 1000mlNH4F into, pour 140mlHF again into, stir and put into the processing of silicon chip heavy metal pollution test reference sheet below 40 minutes.Take out the silicon chip heavy metal pollution test reference sheet of having handled, pure water rinsing, drying are tested with SPV.
Embodiment five
Get a reparative regeneration container, pour 1000mlNH4F into, pour 170mlHF again into, stir and put into the processing of silicon chip heavy metal pollution test reference sheet below 40 minutes.Take out the silicon chip heavy metal pollution test reference sheet of having handled, pure water rinsing, drying are tested with SPV.
Embodiment six
Get a reparative regeneration container, pour 1000mlNH4F into, pour 200mlHF again into, stir and put into the processing of silicon chip heavy metal pollution test reference sheet below 40 minutes.Take out the silicon chip heavy metal pollution test reference sheet of having handled, pure water rinsing, drying are tested with SPV.
Test reference sheet in the foregoing description four～six is measured the result with the processing back and is gathered as follows before processing:
Embodiment seven
Get a reparative regeneration container, pour 1000ml water into, pour the 230mlHF solution stirring again into and evenly put into the processing of silicon chip heavy metal pollution test reference sheet below 40 minutes.Take out the silicon chip heavy metal pollution test reference sheet of having handled, pure water rinsing, drying are tested with SPV.
Embodiment eight
Get a reparative regeneration container, pour 1000ml water into, pour the 265mlHF solution stirring again into and evenly put into the processing of silicon chip heavy metal pollution test reference sheet below 40 minutes.Take out the silicon chip heavy metal pollution test reference sheet of having handled, pure water rinsing, drying are tested with SPV.
Embodiment nine
Get a reparative regeneration container, pour 1000ml water into, pour the 300mlHF solution stirring again into and evenly put into the processing of silicon chip heavy metal pollution test reference sheet below 40 minutes.Take out the silicon chip heavy metal pollution test reference sheet of having handled, pure water rinsing, drying are tested with SPV.
Test reference sheet in the foregoing description seven～nine is measured the result with the processing back and is gathered as follows before processing:
The present invention can not accurately measure or equipment withdraw from service situation after present SPV reference plate is polluted in order to solve; According to the chemical characteristic of silicon single crystal, the test philosophy of SPV body metallic test equipment; Consult silicon single crystal body metallic test standard, and related data, through repetition test, carry out test comparison with existing test reference sheet; Draw above-mentioned prescription and method; The foregoing description result shows reparative regeneration solution and the reparative regeneration method through silicon chip heavy metal pollution test reference sheet of the present invention, can silicon chip heavy metal pollution test reference sheet reparative regeneration not only have been solved the problem of processing and utilizing again after the test reference sheet pollutes; Fully satisfy proper testing and use, and greatly reduce the test and the manufacturing cost of enterprise.
To sum up; The reparative regeneration method design of silicon chip heavy metal pollution test reference sheet of the present invention is unique, and easy and simple to handle, effect is remarkable; Can solve the problem of processing and utilizing again after the test reference sheet pollutes; Fully satisfy proper testing and use, and can reduce the test and the manufacturing cost of enterprise greatly, be suitable for large-scale promotion application.
In this specification, the present invention is described with reference to its certain embodiments.But, still can make various modifications and conversion obviously and not deviate from the spirit and scope of the present invention.Therefore, specification and accompanying drawing are regarded in an illustrative, rather than a restrictive.
Claims (2)
1. the reparative regeneration solution of a silicon chip heavy metal pollution test reference sheet, it is characterized in that: comprise A solution and D solution, said A solution is the hydrogen peroxide of 30wt%, and said D solution is that Potassium aluminum sulfate dodecahydrate is at H
2SO
4In lysate, the said H of 100ml wherein
2SO
4In be dissolved with the said Potassium aluminum sulfate dodecahydrate of 0.15～0.21g.
2. the reparative regeneration method of a silicon chip heavy metal pollution test reference sheet is characterized in that, comprises the following steps:
A) A solution is placed reparative regeneration vessel in heating to 70～80 ℃; Add D solution; Put into said silicon chip heavy metal pollution test reference sheet then and handled 10～40 minutes, wherein said A solution is the hydrogen peroxide of 30wt%, and said D solution is that Potassium aluminum sulfate dodecahydrate is at H
2SO
4In lysate, the said H of 100ml wherein
2SO
4In be dissolved with the said Potassium aluminum sulfate dodecahydrate of 0.15～0.21g;
B) take out the said silicon chip heavy metal pollution test reference sheet of having handled, then with pure water rinsing and dry.
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| CN103983540B (en) * | 2014-05-13 | 2016-03-16 | 北京七星华创电子股份有限公司 | A kind of method judging body iron test value confidence level |
| 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 |
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Effective date of registration: 20191220 Address after: 200444 Building 1, No. 181, Shanlian Road, Baoshan District, Shanghai Patentee after: Shanghai xinxinjingyuan Semiconductor Technology Co., Ltd Address before: 200444 Baoshan District, Baoshan City Industrial Park Road, No., Hill Road, No. 181 Patentee before: Shanghai Shenhe Thermo-magenetic Electronic Co., Ltd. |
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Address after: 200444 Building 1, 181 Shanlian Road, Baoshan District, Shanghai Patentee after: Shanghai Zhongxin wafer semiconductor technology Co.,Ltd. Address before: 200444 Building 1, 181 Shanlian Road, Baoshan District, Shanghai Patentee before: Shanghai xinxinjingyuan Semiconductor Technology Co.,Ltd. |