CN112485528A - Resistance measuring method of high-resistance sheet - Google Patents
Resistance measuring method of high-resistance sheet Download PDFInfo
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- CN112485528A CN112485528A CN202011266350.4A CN202011266350A CN112485528A CN 112485528 A CN112485528 A CN 112485528A CN 202011266350 A CN202011266350 A CN 202011266350A CN 112485528 A CN112485528 A CN 112485528A
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000004140 cleaning Methods 0.000 claims abstract description 22
- 239000000523 sample Substances 0.000 claims abstract description 21
- 238000002161 passivation Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 25
- 238000010301 surface-oxidation reaction Methods 0.000 claims description 12
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 238000000691 measurement method Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000005259 measurement Methods 0.000 abstract description 5
- 150000002500 ions Chemical class 0.000 abstract description 3
- 239000000725 suspension Substances 0.000 abstract description 3
- 238000007669 thermal treatment Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 5
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
- G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Testing Or Measuring Of Semiconductors Or The Like (AREA)
Abstract
The invention discloses a resistance measuring method of a high-resistance sheet, which comprises the following steps: (1) carrying out rapid heat treatment on the high-resistance sheet; (2) carrying out pretreatment before passivation on the high-resistance sheet obtained after the treatment in the step (1); (3) cleaning the high-resistance sheet obtained after the treatment in the step (2); (4) passivating the high-resistance sheet obtained after the treatment in the step (3); (5) and (4) measuring the resistance value of the high-resistance sheet obtained in the step (4) by using a four-probe method. According to the invention, charged ions are injected into the high-resistance sheet oxide layer to neutralize electrons generated in the oxide layer, so that the influence of charged suspension bonds in the natural oxide layer on the measurement of the high-resistance sheet resistance is avoided, and the high-resistance sheet resistance is measured more accurately.
Description
Technical Field
The invention belongs to the technical field of high-resistance sheets, and relates to a resistance measuring method of a high-resistance sheet.
Background
Electronic grade single crystal silicon is an important component of crystal materials and is at the front of the development of new materials. The solar photovoltaic power generation and heat supply semiconductor material is mainly used as a semiconductor material and utilizes solar photovoltaic power generation, heat supply and the like. Various crystal materials, particularly high-tech added-value materials represented by monocrystalline silicon and the development of related high-tech industries become pillars of the contemporary information technology industry, and make the information industry the fastest growing leading industry in the global economic development. Single crystal silicon has great potential, and high-tech resources to be developed and utilized are attracting more and more attention.
Resistance is one of important parameters of silicon single crystals, but in resistance measurement, particularly for high-resistance single crystals, test data are often unstable and have poor repeatability, usually over 10%, which brings many difficulties to production and inspection. In addition to the reason for non-uniformity of single crystal material, the test method is also an important factor affecting data stability and reproducibility.
At present, the resistance measurement method of the monocrystalline silicon wafer is mainly divided into a non-contact type and a contact type. The non-contact measuring resistor such as the eddy current method does not need to contact with a measured object, and cannot cause pollution, but the measuring range is limited, and the non-contact measuring resistor is not suitable for high-resistance measurement. Therefore, the high-resistance sheet measuring resistance mostly adopts a contact type, such as a four-probe measuring method, the measuring range of the method is large, and the high resistance can be measured.
The measured resistance depends on the freely movable particles in the sample, while very few ions are freely movable in the high-resistance sheet. When the high-resistance sheet is exposed to air at room temperature, the surface of the high-resistance sheet is oxidized, and the thin oxide layer is called a natural oxide layer. The existence of the charged dangling bond in the oxide layer will affect the resistance of the high-resistance sheet, and the actual resistance of the high-resistance sheet is difficult to accurately measure due to the influence of the charged dangling bond.
Disclosure of Invention
The invention aims to provide a resistance measuring method of a high-resistance sheet, which aims to solve the problem that the resistance of the high-resistance sheet is influenced by a charged dangling bond in a natural oxide layer.
In order to achieve the purpose, the invention adopts the technical scheme that:
a resistance measurement method of a high-resistance sheet comprises the following steps:
(1) carrying out rapid heat treatment on the high-resistance sheet;
(2) carrying out pretreatment before passivation on the high-resistance sheet obtained after the treatment in the step (1);
(3) cleaning the high-resistance sheet obtained after the treatment in the step (2);
(4) passivating the high-resistance sheet obtained after the treatment in the step (3);
(5) and (4) measuring the resistance value of the high-resistance sheet obtained in the step (4) by using a four-probe method.
In the step (1), the temperature of the rapid heat treatment is 150-1250 ℃, the heating rate is 100-200 ℃/s, and the heat preservation time is 20-50 s.
In the step (2), the pretreatment before passivation is to place the high-resistance sheet in pretreatment liquid, wherein the pretreatment liquid is HF solution or HF solution and HNO3The solution is mixed in any proportion.
For the high-resistance sheet with rough surface, the high-resistance sheet is placed in HF solution and HNO3Soaking in a mixed solution of the HF solution for 1-5 min, wherein the mass concentration of the HF solution is 5%, and the HNO is3The mass concentration of the solution was 95%.
And (3) soaking the high-resistance sheet subjected to surface polishing treatment in an HF solution for 0.5-10 min, wherein the mass concentration of the HF solution is 5%.
In the step (3), the cleaning medium is high-purity water, the cleaning time is not less than 30s, and the cleaning temperature is 50-70 ℃.
In the step (3), the cleaning mode adopts overflow type ultrasonic cleaning.
In the step (4), the passivation treatment is to continuously apply positive/negative charges to the surface oxidation film of the resistor disc obtained in the step (3) by using a corona method, and the applied charges are opposite to the charged type in the surface oxidation film of the resistor disc.
In the step (4), the density of the charge applied by the corona is obtained by measuring the relation between the minority carrier lifetime of the silicon wafer and the density of the corona charge.
The principle of the invention is as follows: the high-resistance sheet is subjected to simple passivation treatment, charged ions are injected into the high-resistance sheet oxide layer, electrons generated in the oxide layer are neutralized, and therefore the influence of charged suspension keys in a natural oxide layer on the resistance measurement of the high-resistance sheet is avoided.
Has the advantages that: according to the invention, the influence of the electrified suspension key in the natural oxidation layer of the high-resistance sheet on resistance measurement is avoided by passivating the high-resistance sheet, so that the resistance of the high-resistance sheet can be measured more accurately. The high-resistance sheet measuring method is simple and rapid to operate, convenient to obtain materials, greatly saves the measuring cost, and can meet the requirements of daily research and industrial manufacturing.
Detailed Description
The invention discloses a method for measuring high-resistance sheet resistance, which comprises the following steps:
(1) and (3) placing the measured high-resistance sheet sample in an RTP-300 type rapid thermal treatment furnace, and performing rapid thermal treatment (RTP) on the sample, wherein the temperature of the rapid thermal treatment is 150-1250 ℃, the temperature rise speed is 100-200 ℃/s, and the heat preservation time is 20-50 s.
(2) Pretreating the high-resistance sheet obtained in the step (1) before passivation, adopting different pretreatment modes according to different surface roughness degrees of the high-resistance sheet, and placing the high-resistance sheet with the rough surface in HF solution with the mass concentration of 5% and HNO with the mass concentration of 95%3Soaking the mixture of the solutions for 1-5 min; and (3) soaking the high-resistance sheet subjected to surface polishing treatment in an HF solution with the mass concentration of 5% for 0.5-10 min.
(3) And (3) cleaning the high-resistance sheet obtained in the step (2) in an ultrasonic cleaning machine, wherein the cleaning medium is high-purity water, the cleaning time is not less than 30s, the cleaning temperature is 50-70 ℃, and the cleaning mode adopts overflow type ultrasonic cleaning.
(4) And (3) continuously applying positive/negative charges to the surface oxidation film of the high-resistance sheet obtained in the step (3) by using a corona (corona) method, wherein the applied charges are opposite to the charged types in the surface oxidation film of the resistance sheet (if the oxidation film is positively charged, negative charges are applied), and thus the passivation treatment is completed.
The corona method is used to inject the appropriate charge to ensure the passivation effect is achieved and the charge density of the corona application is obtained by measuring the relationship between the minority carrier lifetime of the wafer and the corona charge density.
(5) And (4) connecting the circuits according to a measuring principle, and measuring the resistance value of the high-resistance sheet sample obtained in the step (4) by using a four-probe method.
The present invention is further illustrated by the following specific examples.
Example 1
The polished high-resistance sheet resistance is measured, and the thickness of the natural oxide layer is
The specific steps of measuring the resistance of the high-resistance sheet are as follows:
(1) and (3) placing the measured high-resistance sheet sample in an RTP-300 type rapid thermal treatment furnace, and performing rapid thermal treatment on the sample at the temperature of 900 ℃, at the temperature rise speed of 150 ℃/s and at the temperature of 30 s.
(2) And (2) soaking the high-resistance sheet sample obtained in the step (1) for 30s by using an HF solution with the mass concentration of 5%.
(3) And (3) placing the high-resistance sheet obtained in the step (2) in an ultrasonic cleaning machine, and performing overflow type ultrasonic cleaning for 30s by taking high-purity water as a cleaning medium, wherein the cleaning temperature is 50 ℃.
(4) And (4) continuously applying positive/negative charges to the surface oxidation film of the high-resistance sheet obtained in the step (3) by using a corona (corona) method, wherein the applied charges are opposite to the charged type in the surface oxidation film of the resistance sheet, and thus, the passivation treatment is completed. The charge density of the corona application was obtained by measuring the relationship of minority carrier lifetime of the silicon wafer to the corona charge density.
(5) Connecting the circuits according to the measuring principle, and measuring the resistance value of the high-resistance sheet obtained in the step (4) by using a four-probe method.
Example 2
The polished high-resistance sheet resistance is measured, and the thickness of the natural oxide layer is
The method comprises the following specific steps:
(1) and (3) placing the measured high-resistance sheet sample in an RTP-300 type rapid thermal treatment furnace, and performing rapid thermal treatment on the sample at the temperature of 1000 ℃, the temperature rise speed of 160 ℃/s and the heat preservation time of 30 s.
(2) And (2) soaking the high-resistance sheet sample obtained in the step (1) for 6min by using an HF solution with the mass concentration of 5%.
(3) And (3) placing the high-resistance sheet obtained in the step (2) in an ultrasonic cleaning machine, and performing overflow type ultrasonic cleaning for 35s by taking high-purity water as a cleaning medium, wherein the cleaning temperature is 60 ℃.
(4) And (4) continuously applying positive/negative charges to the surface oxidation film of the high-resistance sheet obtained in the step (3) by using a corona (corona) method, wherein the applied charges are opposite to the charged type in the surface oxidation film of the resistance sheet, and thus, the passivation treatment is completed. The charge density of the corona application was obtained by measuring the relationship of minority carrier lifetime of the silicon wafer to the corona charge density.
(5) Connecting the circuits according to the measuring principle, and measuring the resistance value of the high-resistance sheet obtained in the step (4) by using a four-probe method.
Example 3
The method for measuring the resistance of the high-resistance sheet without polishing treatment (rough surface) comprises the following specific steps:
(1) and (3) placing the measured high-resistance sheet sample in an RTP-300 type rapid thermal treatment furnace, and performing rapid thermal treatment on the sample at the temperature of 150 ℃, at the temperature rise speed of 120 ℃/s and at the temperature of 30 s.
(2) Using HF solution with mass concentration of 5% and HNO with mass concentration of 95% for the high-resistance sheet sample obtained in the step (1)3Soaking the mixture solution for 1 min.
(3) And (3) placing the high-resistance sheet obtained in the step (2) in an ultrasonic cleaning machine, and performing overflow type ultrasonic cleaning for 30s by taking high-purity water as a cleaning medium, wherein the cleaning temperature is 60 ℃.
(4) And (4) continuously applying positive/negative charges to the surface oxidation film of the high-resistance sheet obtained in the step (3) by using a corona (corona) method, wherein the applied charges are opposite to the charged type in the surface oxidation film of the resistance sheet, and thus, the passivation treatment is completed. The charge density of the corona application was obtained by measuring the relationship of minority carrier lifetime of the silicon wafer to the corona charge density.
(5) Connecting the circuits according to the measuring principle, and measuring the resistance value of the high-resistance sheet obtained in the step (4) by using a four-probe method.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (9)
1. A resistance measurement method of a high-resistance sheet is characterized in that: the method comprises the following steps:
(1) carrying out rapid heat treatment on the high-resistance sheet;
(2) carrying out pretreatment before passivation on the high-resistance sheet obtained after the treatment in the step (1);
(3) cleaning the high-resistance sheet obtained after the treatment in the step (2);
(4) passivating the high-resistance sheet obtained after the treatment in the step (3);
(5) and (4) measuring the resistance value of the high-resistance sheet obtained in the step (4) by using a four-probe method.
2. The method for measuring the resistance of the high-resistance sheet according to claim 1, characterized in that: in the step (1), the temperature of the rapid heat treatment is 150-1250 ℃, the heating rate is 100-200 ℃/s, and the heat preservation time is 20-50 s.
3. The method for measuring the resistance of the high-resistance sheet according to claim 1, characterized in that: in the step (2), the pretreatment before passivation is to place the high-resistance sheet in pretreatment liquid, wherein the pretreatment liquid is HF solution or HF solution and HNO3The solution is mixed in any proportion.
4. The method for measuring the resistance of a high resistance sheet according to claim 3, characterized in that: for the high-resistance sheet with rough surface, the high-resistance sheet is placed in HF solution and HNO3Soaking in a mixed solution of the HF solution for 1-5 min, wherein the mass concentration of the HF solution is 5%, and the HNO is3The mass concentration of the solution was 95%.
5. The method for measuring the resistance of a high resistance sheet according to claim 3, characterized in that: and (3) soaking the high-resistance sheet subjected to surface polishing treatment in an HF solution for 0.5-10 min, wherein the mass concentration of the HF solution is 5%.
6. The method for measuring the resistance of the high-resistance sheet according to claim 1, characterized in that: in the step (3), the cleaning medium is high-purity water, the cleaning time is not less than 30s, and the cleaning temperature is 50-70 ℃.
7. The resistance measurement method of the high resistance sheet according to claim 1 or 6, characterized in that: in the step (3), the cleaning mode adopts overflow type ultrasonic cleaning.
8. The method of measuring high resistance sheet resistance according to claim 1, characterized in that: in the step (4), the passivation treatment is to continuously apply positive/negative charges to the surface oxidation film of the resistor disc obtained in the step (3) by using a corona method, and the applied charges are opposite to the charged type in the surface oxidation film of the resistor disc.
9. The method of measuring high resistance sheet resistance according to claim 8, characterized in that: in the step (4), the density of the charge applied by the corona is obtained by measuring the relation between the minority carrier lifetime of the silicon wafer and the density of the corona charge.
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