CN108344774A - The impurity concentration detection method of ultra-pure germanium stick or ingot - Google Patents
The impurity concentration detection method of ultra-pure germanium stick or ingot Download PDFInfo
- Publication number
- CN108344774A CN108344774A CN201710054354.8A CN201710054354A CN108344774A CN 108344774 A CN108344774 A CN 108344774A CN 201710054354 A CN201710054354 A CN 201710054354A CN 108344774 A CN108344774 A CN 108344774A
- Authority
- CN
- China
- Prior art keywords
- germanium
- stick
- ingot
- impurity concentration
- ultra
- 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
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/041—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Testing Or Measuring Of Semiconductors Or The Like (AREA)
Abstract
The present invention provides the impurity concentration detection methods of a kind of ultra-pure germanium stick or ingot, and using two sonde method checked for impurities concentration of direct current, the germanium stick or ingot are detected under 77K constant temperature；Any measurement point of the germanium stick or ingot radical length is coated with indium gallium alloy；The equidistant voltage drop U that two probe measures, passes through functional relationElectricalresistivityρ is calculated, further according to functional relation n=1/ (ρ × q × μ), the average net impurity concentration n of the germanium stick between probe pen or ingot is calculated.Method provided by the invention solves the problems, such as that the whole impurity concentration of germanium stick or ingot can not be detected at present, ensure the integrality of sample to be tested, testing result is accurate, and detection efficiency is high, is conducive to industrialization.
Description
Technical field
The present invention relates to the impurity concentrations of semiconductor Germanium stick or ingot detection field more particularly to a kind of ultra-pure germanium stick or ingot
Detection method.
Background technology
Germanium product currently on the market is usually finally to be reached by pulling monocrystal again through zone-refine after chemical purification
To the purity of 5~6N, due to the impurity content less than the germanium sample of 6N purity have with its room temperature (23 ± 5 DEG C) resistivity it is certain right
It should be related to, therefore the testing requirements of the purity germanium product are mainly electrical property at present, i.e. the size of resistivity.
It is usually to measure its body electricity using two probe resistance rate detection methods under room temperature (23 ± 5 DEG C) to melt germanium ingot for area
Resistance, the relevant criterion of existing two probe resistance rate detection methods domestic at present：YS/T602 2007《Melt germanium ingot resistivity measurement in area
Two sonde method of method》；Germanium single crystal stick for drawing is usually that four probe resistance rate detection sides are used under room temperature (23 ± 5 DEG C)
Method measures the sheet resistance rate on section, the relevant criterion of existing four probe resistance rate detection methods domestic at present：GB/T
26074 2010《Germanium single crystal resistivity direct current four-point probe measurment method》.
But for the HpGe product of higher purity or even 12~13N, resistivity at room temperature infinite approach intrinsic resistivity
48 Ω cm, test resistance rate can not accurately differentiate its specific purity under room temperature.The miscellaneous of 12~13N ultra-pure germaniums is measured at present
Matter concentration, what is taken is germanium flake progress low temperature (77K) Hall detection to thickness less than 1mm, and the carrier concentration measured is i.e.
For its impurity concentration.Low temperature Hall detection method proposed by Van der pauw in 1958 at first, not by long-run development
It is disconnected to tend to be perfect, it is domestic at present to have ripe Hall examination criteria：GB/T 4326-2006《Extrinsic semiconductor monocrystalline Hall
Mobility and Hall effect measurement method》.But single low temperature Hall detection method is only applicable to test laminar sample, for
Crystal bar, it is necessary to which pair cross-section is sliced and cleans rear and can measure, and efficiency is too low, and chooses when being sliced point without objective basis, band
There is certain blindness.Therefore, the detection of low temperature Hall is feasible as a kind of confirmatory survey eventually, but can not be to rodlike or ingot shape
The whole impurity concentration of ultra-pure germanium product be detected.
Therefore, there is an urgent need for a kind of methods for the whole impurity concentration that can detect ultra-pure germanium product.
Invention content
In order to overcome above-mentioned the shortcomings of the prior art and disadvantage, the present invention provides a kind of ultra-pure germanium stick or ingots
Impurity concentration detection method can detect the whole impurity of sample to be tested under the premise of ensureing sample to be tested integrality
Concentration.
To realize that foregoing purpose, the present invention adopt the following technical scheme that：A kind of inspection of the impurity concentration of ultra-pure germanium stick or ingot
Survey method, using two sonde method checked for impurities concentration of direct current, the germanium stick or ingot are detected under 77K constant temperature；The germanium stick
Or any measurement point of the radical length of ingot coats indium gallium alloy；The equidistant voltage drop U that two probe measures, passes through function
Relational expressionIt is calculated electricalresistivityρ, in formula, I is the electric current by germanium stick to be measured or ingot；S be germanium stick to be measured or
The cross-sectional area of ingot；L is probe spacing；
Further according to functional relation n=1/ (ρ × q × μ), the average net impurity of the germanium stick between probe pen or ingot is calculated
Concentration n；In formula, q is unit charge amount 1.602 × 10-19C；μ is the intrinsic mobility of germanium, is 40000cm under 77K2/(V·
s)。
As a further improvement on the present invention, the spacing of the adjacent measurement points of the germanium stick or ingot surface is 0.5~2cm.
As a further improvement on the present invention, the indium gallium alloy of the coating is in filament form.
As a further improvement on the present invention, the dedicated microprocessor of the detection method can be according to functional relation：With n=1/ (ρ × q × μ), output indicates net impurity concentration and germanium stick or point of ingot radical length with logarithmic coordinates
Cloth curve.
As a further improvement on the present invention, the radial cross-sectional area of the germanium stick or ingot remains unchanged or linearly becomes
Change.
The present invention is detected the whole impurity concentration of germanium stick or ingot using two sonde methods, is waited under the liquid nitrogen temperature of 77K
Detection germanium stick or ingot indicate net impurity concentration and germanium stick or the distribution curve of ingot radical length with logarithmic coordinates, solve current nothing
Method detects the problem of ultra-pure germanium stick or ingot entirety Impurity Distribution.The present invention is coated with indium in probe and germanium stick or ingot surface contact position
Gallium alloy makes measurement voltage more stablize to form Ohmic contact.Detection method provided by the invention, it is easy to operate, it measures accurate
Really, detection efficiency is high.
Description of the drawings
Fig. 1 is that Ge-1 germanium stick indicates net impurity concentration n (ordinate) along germanium stick radical length (abscissa) with logarithmic coordinates
Scatter chart.
Wherein, curve a indicates measurement result under forward current；Curve b indicates measurement result under reverse current.
Specific implementation mode
Technical solution is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
The every other embodiment that technical staff is obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention adopts the following technical scheme that：The impurity concentration detection method of a kind of ultra-pure germanium stick or ingot, using direct current
Two sonde method checked for impurities concentration, germanium stick or ingot are detected under 77K constant temperature；Any measurement of the radical length of germanium stick or ingot
Point coating indium gallium alloy；The equidistant voltage drop U that two probes measure, passes through functional relationResistance is calculated
Rate ρ, in formula, I is the electric current by germanium stick to be measured or ingot；S is the cross-sectional area of germanium stick or ingot to be measured；L is probe spacing；
Further according to functional relation n=1/ (ρ × q × μ), the average net impurity of the germanium stick between probe pen or ingot is calculated
Concentration n；In formula, q is unit charge amount 1.602 × 10-19C；μ is the intrinsic mobility of germanium, is 40000cm under 77K2/(V·
s)。
In the present invention, any measurement point of the radical length of germanium stick or ingot coats indium gallium alloy, so as to probe and germanium stick or
Ohmic contact is formed between ingot, measurement voltage is made more to stablize, it is preferred that the indium gallium alloy coated on germanium stick or ingot is in filament shape
Formula, filament is elongated as possible, and thickness is small as possible.
Two ends of germanium stick or ingot radial direction can be connected by the scale copper of winding with constant-current source, then germanium stick or ingot are put
Set on supporting rack, makes liquid nitrogen flood germanium stick or ingot in the open liquid nitrogen tank equipped with liquid nitrogen, is 77K permanent to ensure to detect temperature
Temperature.
In the present invention, constant-current source is capable of providing the DC power supply of 0.01~100mA, and when measurement shows electric current, and can
It adjusts；The measurement range for the voltmeter being connect with two probes is 0.01~1000mV, and when measurement, voltage value can be shown.
In the present invention, functional relation is incorporated into dedicated microprocessorIt, will be each with n=1/ (ρ × q × μ)
A parameter value is input on dedicated microprocessor, so that it may obtain germanium stick or ingot with logarithmic coordinates indicate net impurity concentration and germanium stick or
The distribution curve of ingot radical length.
Embodiment 1 provided by the invention provides constant-current source using model KDB-1A impurity concentration detectors, and can be automatic
The equidistant voltage that record, transmission probe measure drops on dedicated microprocessor.
The method of the present invention is specifically introduced below in conjunction with embodiment 1.
Embodiment 1.
Detection number is that the radical length of Ge-1 germanium sticks is 33cm, and a diameter of 2.29cm is dense using model KDB-1A impurity
It spends detector and constant-current source is provided, and pass through the voltage between the included adjacent measurement point of two probe in detecting of impurity concentration detector
Drop, shows and is transmitted on dedicated microprocessor.
1) indium gallium alloy is dipped with paintbrush brush, indium gallium alloy, the indium of coating is coated every 1cm along germanium stick radical length surface
Gallium alloy filament need to be elongated as possible, thin as possible.
2) radial two ends of the germanium stick for coating indium gallium alloy are connected to the constant current of model KDB-1A impurity concentration detectors
On source：It is 0.02~0.1mm with thickness, width is 5~10mm and copper sheet with holes winds germanium stick both ends, and by copper derived from constant-current source
Conducting wire passes through copper sheet hole and winds securely, and copper sheet is made to be anchored on germanium stick both ends, until the electric current of display keeps stablizing.
3) germanium stick supporting rack is placed in liquid nitrogen tank, and fills liquid nitrogen in liquid nitrogen tank.
4) germanium stick is slowly placed on the supporting rack in liquid nitrogen tank, so that liquid nitrogen is submerged germanium stick, and make germanium stick at low temperature
Electric current keeps stablizing.
5) it is passed through forward current, when measurement, one holds a probe pen, according to the position of coating indium gallium alloy, every 1cm
By the pressing of probe pen tip on germanium stick surface, after measurement voltage stabilization to be shown, inspires software and read measurement data；Change electricity
Direction is flowed, then is remeasured, measurement data is read.
6) export net impurity concentration n after measuring, and in a manner of logarithmic coordinates come show net impurity concentration n (containing time
Number formulary) along the distribution curve of germanium stick length.
Dedicated microprocessor is incorporated into functional relationWith n=1/ (ρ × q × μ), pass through each ginseng of input
Numerical value obtains indicating that net impurity concentration n (ordinate) is bent along the distribution in germanium stick radical length direction (abscissa) with logarithmic coordinates
Line, as shown in Fig. 1.
Using GB/T 4326-2006《Extrinsic semiconductor monocrystalline hall mobility and Hall effect measurement method》,
The 11st point that number is Ge-1 germanium sticks surface is measured under 77K constant temperature, i.e., abscissa is that the impurity of the germanium stick at 11cm is dense in attached drawing 1
Degree, testing result are shown in table 1.
Impurity concentration result at confirmatory the 11st point of detection Ge-1 germanium sticks surface of table 1
Known by table 1, using GB/T 4326-2006《Extrinsic semiconductor monocrystalline hall mobility and Hall effect measurement side
Method》Impurity concentration at the 11st point of Ge-1 germanium sticks surface is detected under the constant temperature of 77K, the forward current and reverse current the case where
Under, which is (1~4) × 1011/cm3, with reference to the accompanying drawings 1 it is found that the 11st point in forward current and reverse current
Under, carrier concentration (net impurity concentration) is (2~3) × 1011/cm3, testing result is consistent, it was demonstrated that method detection of the invention
Accurately.
Detection method provided by the invention detects the whole of ultra-pure germanium stick or ingot in a low temperature of 77K using two sonde methods
Body impurity concentration solves the problems, such as that the whole impurity concentration of germanium stick or ingot can not be detected at present, ensure that the complete of sample to be tested
Whole property, while using GB/T 4326-2006《Extrinsic semiconductor monocrystalline hall mobility and Hall effect measurement method》
It is verified under the constant temperature of 77K, it was demonstrated that testing result of the present invention is accurate.Method detection efficiency provided by the invention is high, is conducive to industry
Change.
Although being example purpose, the preferred embodiment of the present invention, the ordinary skill people of this field are had been disclosed for
Member will realize in the case where not departing from the scope and spirit of the present invention disclosed in appended claims, various to change
Into, increase and substitution be possible.
Claims (5)
1. the impurity concentration detection method of a kind of ultra-pure germanium stick or ingot, special using two sonde method checked for impurities concentration of direct current
Sign is：
The germanium stick or ingot are detected under 77K constant temperature；
Any measurement point of the radical length of the germanium stick or ingot coats indium gallium alloy；
The equidistant voltage drop U that two probe measures, passes through functional relation
It is calculated electricalresistivityρ, in formula, I is the electric current by germanium stick to be measured or ingot；S is the cross section face of germanium stick or ingot to be measured
Product；L is probe spacing；
Further according to functional relation, the average net impurity that the germanium stick between probe pen or ingot is calculated is dense
Spend n；In formula, q is unit charge amount 1.602 × 10-19C；μ is the intrinsic mobility of germanium, is 40000 cm under 77K2/（V·
s）.
2. the impurity concentration detection method of ultra-pure germanium stick according to claim 1 or ingot, it is characterised in that：The germanium
The spacing of the adjacent measurement points of stick or ingot surface is 0.5 ~ 2 cm.
3. the impurity concentration detection method of ultra-pure germanium stick according to claim 1 or ingot, it is characterised in that：The coating
Indium gallium alloy be in filament form.
4. the impurity concentration detection method of ultra-pure germanium stick according to claim 1 or ingot, it is characterised in that：The detection
The dedicated microprocessor of method can be according to functional relation：WithOutput is with logarithmic coordinates
Indicate net impurity concentration and germanium stick or the distribution curve of ingot radical length.
5. the impurity concentration detection method of ultra-pure germanium stick according to claim 1 or ingot, it is characterised in that：The germanium stick
Or the radial cross-sectional area of ingot remains unchanged or linear change.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710054354.8A CN108344774A (en) | 2017-01-22 | 2017-01-22 | The impurity concentration detection method of ultra-pure germanium stick or ingot |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710054354.8A CN108344774A (en) | 2017-01-22 | 2017-01-22 | The impurity concentration detection method of ultra-pure germanium stick or ingot |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108344774A true CN108344774A (en) | 2018-07-31 |
Family
ID=62962870
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710054354.8A Pending CN108344774A (en) | 2017-01-22 | 2017-01-22 | The impurity concentration detection method of ultra-pure germanium stick or ingot |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108344774A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111060564A (en) * | 2019-10-27 | 2020-04-24 | 山西子盟科技开发有限公司 | Device and method for detecting purity of gold brick through resistivity |
| CN111060563A (en) * | 2019-10-27 | 2020-04-24 | 山西子盟科技开发有限公司 | Device and method for identifying gold brick doping through resistivity |
| CN114235899A (en) * | 2021-12-16 | 2022-03-25 | 安徽光智科技有限公司 | Method for detecting carrier concentration of ultra-high-purity germanium single crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401999A (en) * | 2002-09-10 | 2003-03-12 | 西安电子科技大学 | Strain Si-Ge film material doped concentration testing method |
| CN103048360A (en) * | 2012-11-30 | 2013-04-17 | 西安隆基硅材料股份有限公司 | Method for measuring concentration of germanium or/and tin impurity in crystalline silicon |
-
2017
- 2017-01-22 CN CN201710054354.8A patent/CN108344774A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401999A (en) * | 2002-09-10 | 2003-03-12 | 西安电子科技大学 | Strain Si-Ge film material doped concentration testing method |
| CN103048360A (en) * | 2012-11-30 | 2013-04-17 | 西安隆基硅材料股份有限公司 | Method for measuring concentration of germanium or/and tin impurity in crystalline silicon |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111060564A (en) * | 2019-10-27 | 2020-04-24 | 山西子盟科技开发有限公司 | Device and method for detecting purity of gold brick through resistivity |
| CN111060563A (en) * | 2019-10-27 | 2020-04-24 | 山西子盟科技开发有限公司 | Device and method for identifying gold brick doping through resistivity |
| CN111060564B (en) * | 2019-10-27 | 2023-05-09 | 山西子盟科技开发有限公司 | Device and method for detecting purity of gold brick through resistivity |
| CN111060563B (en) * | 2019-10-27 | 2023-05-09 | 山西子盟科技开发有限公司 | Device and method for identifying doping of gold bricks through resistivity |
| CN114235899A (en) * | 2021-12-16 | 2022-03-25 | 安徽光智科技有限公司 | Method for detecting carrier concentration of ultra-high-purity germanium single crystal |
| CN114235899B (en) * | 2021-12-16 | 2023-11-03 | 安徽光智科技有限公司 | Method for detecting carrier concentration of ultra-high purity germanium single crystal |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108344774A (en) | The impurity concentration detection method of ultra-pure germanium stick or ingot | |
| CN104931335B (en) | Conducting function material stress-electric coupling effect test system and its method of testing | |
| CN108572195A (en) | A kind of method and device measuring the plant physiology impedance under specific chucking power | |
| CN109752416A (en) | Slurry uniformity detection method and application | |
| CN204631135U (en) | A kind of aqueous solution conductivity detector | |
| CN201562017U (en) | Portable device for quickly measuring conductor conductivity | |
| CN206114470U (en) | Lithium ion battery diaphragm moisture absorption speed testing arrangement | |
| CN202994906U (en) | An apparatus having four probes for measuring resistivity of graphite fibers | |
| CN211453441U (en) | Resistivity test device under tensile state of indoor undisturbed soil sample | |
| CN202018493U (en) | Tweezers type testing device for conduction types of silicon materials | |
| CN205786856U (en) | Device for measuring conductivity of damp surface of contaminated insulator | |
| CN102288933B (en) | Calibration method used for measuring solution conductivity lower than 10mus/cm | |
| CN207366636U (en) | Battery pole piece resistance testing device | |
| CN203324379U (en) | Sample fixing device of DC resistance tester | |
| CN103424629A (en) | Simple method for testing impedance of graphene oxide solution | |
| CN103557952B (en) | Intelligent mercurial thermometer capable of being monitored in real time | |
| CN105092979A (en) | Method for measuring internal resistance of marine Ag/AgCl electric field sensor | |
| CN206248605U (en) | A kind of three-electrode cell | |
| CN108572193A (en) | The assay method and device of a kind of intrinsic transporting power of plant leaf blade based on physiology electric current | |
| CN201373834Y (en) | Online electronic solution concentration meter | |
| CN106353383B (en) | A kind of sensor detecting hexafluorophosphoricacid acid ions | |
| CN203350364U (en) | Universal meter type measuring instrument for detecting amorphous silicon thin film cell panel sheet resistance | |
| CN206523561U (en) | A kind of plain type resistivity detecting device | |
| CN205280917U (en) | Flexible graphite alkene nanometer wall magnetic field detection device | |
| CN202929112U (en) | Apparatus for testing resistivity of solar cell material under low temperature |
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 |
Effective date of registration: 20190603 Address after: 511517 27-9B, Guangdong Qingyuan hi tech Industrial Park Applicant after: Guangdong forerunner materials Limited by Share Ltd Address before: 511517 27-9B, Guangdong Qingyuan hi tech Industrial Park Applicant before: Qingyuan Xiandao Materials Co., Ltd. |
|
| TA01 | Transfer of patent application right | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180731 |
|
| RJ01 | Rejection of invention patent application after publication |