CN117831826A - Ca ion generation method suitable for ECR ion source device - Google Patents
Ca ion generation method suitable for ECR ion source device Download PDFInfo
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- CN117831826A CN117831826A CN202311730833.9A CN202311730833A CN117831826A CN 117831826 A CN117831826 A CN 117831826A CN 202311730833 A CN202311730833 A CN 202311730833A CN 117831826 A CN117831826 A CN 117831826A
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- furnace crucible
- induction
- ion source
- ecr
- heating temperature
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- 229910001424 calcium ion Inorganic materials 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000006698 induction Effects 0.000 claims abstract description 51
- 238000010438 heat treatment Methods 0.000 claims abstract description 38
- 150000002500 ions Chemical class 0.000 claims abstract description 37
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 29
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 20
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000292 calcium oxide Substances 0.000 claims abstract description 20
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 239000011575 calcium Substances 0.000 abstract description 23
- 229910052791 calcium Inorganic materials 0.000 abstract description 13
- 238000010884 ion-beam technique Methods 0.000 abstract description 9
- 238000011160 research Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000009467 reduction Effects 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000010405 reoxidation reaction Methods 0.000 abstract description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000011900 installation process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- Electron Sources, Ion Sources (AREA)
Abstract
The invention belongs to the field of rare isotope ion preparation, and particularly relates to a Ca ion generation method suitable for an ECR ion source device, which comprises the following steps: 1) Uniformly mixing calcium oxide powder with a reducing agent to obtain a mixture; 2) Loading the mixture into an induction furnace crucible and installing the induction furnace crucible into a plasma arc chamber of an ECR ion source apparatus; 3) And heating the induction high-temperature furnace crucible to 700-900 ℃, and enabling the generated elemental calcium steam to enter a discharge chamber of the ECR ion source device so as to be ionized to generate the required Ca ions. The method removes the external reduction device, and the whole process is simpler and more controllable; the simple substance calcium steam is produced and used immediately, is not stored, avoids reoxidation, and improves the use efficiency of raw materials; obtained in this way 40 Ca/ 48 The Ca ion beam intensity can reach 2-10pμA, and the experimental requirement of an overweight research device can be met.
Description
Technical Field
The invention belongs to the field of preparation of rare isotope ions, and particularly relates to a Ca ion generation method suitable for an ECR ion source device.
Background
48 Ca is rich in neutronThe lack of isotopes, which are only 0.187% abundant, usually exist in the form of calcium oxide, and are quite expensive. The overweight research device in modern physical research institute requires ECR ion source device capable of providing 2-10puA 48 Ca ion beam. The ECR ion source utilizes electron to generate resonance in the magnetic field with the same convolution frequency as the fed microwave frequency, the electrons with energy are generated into high-charge state ions through gradual collision ionization, and then various charge state ion beams are led out.
Currently, internationally related laboratories (e.g., russian Dubna) offer 48 Ca ions are mainly reduced and then used. Reducing calcium oxide into elemental calcium by using external equipment, storing the elemental calcium, loading the elemental calcium into a crucible of a low-temperature furnace, installing the elemental calcium into an ECR ion source device, heating the elemental calcium to obtain calcium metal steam, and feeding the calcium metal steam into ECR plasma to generate the calcium metal steam 48 Ca ion beam. The method firstly needs a complex set of calcium reduction equipment, and meanwhile, the temperature of the reduction process, the simple substance calcium collection, storage and installation processes are strictly controlled so as to avoid the reoxidation of the simple substance calcium. The reduction efficiency in this manner is typically 50-70%, and a single reduction yields 50-70mg elemental calcium, estimated at a consumption rate of 0.5mg/h, which is maintained for only about 6 days.
Disclosure of Invention
The invention aims to meet the requirement of heavy ion accelerator experiments, in particular to the requirement of overweight research devices of modern physical research institute on rare isotopes 48 The Ca ion generating method is suitable for ECR ion source devices, greatly simplifies the process steps and further improves the utilization efficiency of rare isotope raw materials.
Specifically, the invention provides the following technical scheme:
a Ca ion generation method suitable for use in an ECR ion source apparatus, comprising the steps of:
1) Uniformly mixing calcium oxide powder with a reducing agent to obtain a mixture;
2) Loading the mixture into an induction furnace crucible and installing the induction furnace crucible into a plasma arc chamber of an ECR ion source apparatus;
3) And heating the induction high-temperature furnace crucible to 700-900 ℃, and enabling the generated elemental calcium steam to enter a discharge chamber of the ECR ion source device so as to be ionized to generate the required Ca ions.
According to the invention, the calcium oxide mixture is filled into the induction high-temperature furnace crucible and is arranged in the plasma arc cavity of the ECR ion source device, and the process of reducing the calcium oxide into the elemental calcium and the process of evaporating the elemental calcium into the calcium metal steam are simultaneously carried out by heating the mixture of the calcium oxide and the reducing agent.
In the traditional method, calcium oxide is reduced into elemental calcium by using external equipment at the temperature of more than 1300 ℃, then the elemental calcium is put into a furnace crucible and is arranged in an ECR ion source device, and continuous calcium metal steam is obtained by heating the elemental calcium at the temperature of about 500 ℃ and is fed into ECR plasma so as to generate 48 Ca ion beam. In the invention, if the induction high temperature furnace crucible is heated to more than 1300 ℃ in the step 3), the calcium oxide powder is quickly reduced and further quickly evaporated into simple substance calcium steam, so that the continuous and stable 2-10p mu A Ca ion beam intensity cannot be generated for the ECR ion source to meet the requirement of an overweight research device. The present inventors have unexpectedly found that by mixing a calcium oxide powder with a specific reducing agent and heating the induction furnace crucible to a temperature of 700-900 ℃, a simultaneous slow progress of the reduction process and the evaporation process can be achieved, thus obtaining 40 Ca/ 48 The Ca ion beam intensity can reach 2-10pμA, and the experimental requirement of an overweight research device can be met. If the temperature is lower than the above temperature, for example, a conventional crucible is heated at about 500 ℃, only a small amount of calcium ions are generated, and the experimental requirements cannot be satisfied.
Preferably, in step 1), the reducing agent is aluminum powder and/or zirconium powder. The aluminum powder, the zirconium powder and the generated oxides thereof have higher melting points, no extra steam pollution is generated at the working temperature of 700-900 ℃, and meanwhile, the continuous slow reduction of the calcium oxide can be realized. The mechanism of reducing calcium oxide is as follows:
3CaO+2Al→Al 2 O 3 +3Ca-------(1)
2CaO+2Zr→ZrO 2 +2Ca-------(2)
preferably, in step 1), the reducing agent is added in excess.
Further preferably, in the step 1), the reducing agent is aluminum powder, and the mass ratio of the calcium oxide powder to the aluminum powder is 1:0.35-1:0.4.
Preferably, in step 2), the induction furnace crucible is the device described in chinese patent CN 201920445433.6. The induction high-temperature furnace crucible has the advantages of high working temperature, uniform heating and large volume, thereby achieving the conditions required by reduction reaction and improving single beam-supplying time.
Preferably, the dosage of the calcium oxide powder is 400-600 mg, the induction high temperature furnace crucible is heated in a step manner in the step 3), and the specific steps are as follows:
on days 1-5, the heating temperature of the induction high temperature furnace crucible is 700 ℃;
on day 6, the heating temperature of the induction furnace crucible is increased from 700 ℃ to 750 ℃;
the heating temperature of the induction high-temperature furnace crucible is 750 ℃ in 7-10 days;
on day 11, the heating temperature of the induction furnace crucible is increased from 750 ℃ to 800 ℃;
on the 12 th to 15 th days, the heating temperature of the induction high temperature furnace crucible is 800 ℃;
on day 16, the heating temperature of the induction furnace crucible was increased from 800 ℃ to 850 ℃;
on days 17-19, the heating temperature of the induction high temperature furnace crucible is 850 ℃;
on day 20, the heating temperature of the induction furnace crucible is increased from 850 ℃ to 900 ℃;
on day 21, the induction furnace crucible was heated to 900 ℃.
According to the invention, through the step adjustment (precision +/-1 ℃) of the consumption of the calcium oxide powder and the working temperature of the crucible, the accurate control of the steam quantity of the elemental calcium can be realized, so that ECR ions always work in a relatively stable area, and the fluctuation of the beam current of the Ca ions is less than +/-5%. After the step heating is finished, the residual raw materials are insufficient to support the required beam intensity and stability, and the raw materials of the furnace need to be added.
The invention has the following beneficial effects:
the Ca ion generating method suitable for ECR ion source device can generate the calcium ions required by Lanzhou heavy ion accelerator, especially overweight research device, and simultaneously greatly simplifies the traditional scheme, and improves the utilization efficiency of raw materials, especially rare isotopes.
Using the method of the present invention, 2-10pμA has been successfully obtained at the recent physical institute room temperature ECR ion source LECR5 40 Ca 13+ 2-3eμA 48 Ca 14+ The beam successfully reaches the overweight research terminal.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following description will briefly explain the drawings needed in the embodiments or the prior art, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a typical spectrum of high current calcium ions produced by the method of example 1 of the present invention, wherein the abscissa is the analyzed magnet current in amperes; the ordinate is the calcium ion beam intensity, in electron microamps.
Fig. 2 is a schematic diagram of a method of example 1 according to the present invention for directly heating a calcium oxide + reductant mixture in an ECR ion source apparatus using an induction furnace crucible.
Fig. 3 is a graph showing the beam stability for 7 hours continuously tested according to the method of example 1 of the present invention. Wherein the abscissa is time from 21:30 to 04:30; the ordinate is the intensity of the calcium ion beam, and the unit is electron microamperes.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; the reagents, materials, etc. used in the examples described below are commercially available unless otherwise specified.
For the induction furnace crucible used in the following examples, see CN201920445433.6"ECR ion source induction furnace", published in year 2020, 01, 03, patent application Lu Wang et al, 2019, applicant: modern physical institute of China academy of sciences. For the sake of brevity, only this is cited, but all of the technical disclosures of the above patents should also be considered as part of the technical disclosure of the present application. The induction furnace crucible is heated by an ac power source of 150-200kHz, 0-2.4 kW.
Example 1
Example 1 provides a Ca ion generation method suitable for use in ECR ion source apparatus, with partial reference to fig. 2, comprising the steps of:
1) Uniformly mixing 500mg of calcium oxide powder and 175mg of aluminum powder to obtain a mixture;
2) Loading the mixture into an induction furnace crucible and installing the induction furnace crucible into a plasma arc chamber of an ECR ion source apparatus;
3) Heating the induction high temperature furnace crucible to generate simple substance calcium steam, and enabling the simple substance calcium steam to enter a discharge chamber of the ECR ion source device so as to be ionized to generate required Ca ions; typical heating is as follows, each implementation may vary slightly depending on ECR ion source conditions:
on days 1-5, the heating temperature of the induction high temperature furnace crucible is 700 ℃;
on day 6, the heating temperature of the induction furnace crucible is increased from 700 ℃ to 750 ℃;
the heating temperature of the induction high-temperature furnace crucible is 750 ℃ in 7-10 days;
on day 11, the heating temperature of the induction furnace crucible is increased from 750 ℃ to 800 ℃;
on the 12 th to 15 th days, the heating temperature of the induction high temperature furnace crucible is 800 ℃;
on day 16, the heating temperature of the induction furnace crucible was increased from 800 ℃ to 850 ℃;
on days 17-19, the heating temperature of the induction high temperature furnace crucible is 850 ℃;
on day 20, the heating temperature of the induction furnace crucible is increased from 850 ℃ to 900 ℃;
on day 21, the induction furnace crucible was heated to 900 ℃.
After the step heating is finished, if the heating is continued, the later furnace temperature may exceed 900 ℃ (representing insufficient furnace burden), so that the furnace needs to be replaced or the furnace burden needs to be added in time.
The ECR ion source device has the following working parameters: microwave frequency: 18+14.5GHz, vacuum range: 1.0X10 -8 mbar～5.0×10 -7 mbar。
FIG. 1 is a graph of typical calcium ions in strong current generated by the method of example 1 of the present invention, in this example, the supporting gas is oxygen, the microwave power fed into the source is 1.8+0.2 kilowatts, the ion source is led out at a high voltage of 30.7 kilovolts, and the high voltage is loaded with 2.9 milliamperes of electrons, resulting in a mixed beam of calcium and oxygen, comprising 40 Ca 11+ , 40 Ca 12+ , 40 Ca 13+ ， 16 O 3+ ， 16 O 4+ ， 16 O 5+ Etc. The mixed beam enters an analysis magnet at the rear end to separate ions with different charge-to-mass ratios (M/Q), and finally the required 40 Ca 13+ To a linear accelerator.
FIG. 3 is a rootAccording to the method of example 1 of the present invention, beam stability was continuously tested for 7 hours, and as can be seen, 40 Ca 13+ approximately 100euA (7.69 puA), the ECR ions are always operated in a relatively stable region by precise control of the amount of elemental calcium vapor.
While the invention has been described in detail in the foregoing general description and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (6)
1. A Ca ion generation method suitable for use in an ECR ion source apparatus, comprising the steps of:
1) Uniformly mixing calcium oxide powder with a reducing agent to obtain a mixture;
2) Loading the mixture into an induction furnace crucible and installing the induction furnace crucible into a plasma arc chamber of an ECR ion source apparatus;
3) And heating the induction high-temperature furnace crucible to 700-900 ℃, and enabling the generated elemental calcium steam to enter a discharge chamber of the ECR ion source device so as to be ionized to generate the required Ca ions.
2. The Ca ion generation method according to claim 1, wherein in step 1), the reducing agent is aluminum powder and/or zirconium powder.
3. The Ca ion generation method according to claim 1 or 2, wherein in step 1), the reducing agent is added in excess.
4. The Ca ion generation method according to claim 3, wherein the reducing agent is aluminum powder, and the mass ratio of the calcium oxide powder to the aluminum powder is 1:0.35-1:0.4.
5. The method of claim 1 to 4, wherein in step 2), the induction furnace crucible is an apparatus according to chinese patent CN 201920445433.6.
6. The Ca ion generation method for ECR ion source apparatus according to claims 1 to 5, wherein in step 3), the amount of the calcium oxide powder is 400 to 600mg, and in step 3), the induction high temperature furnace crucible is heated by steps, comprising the steps of:
on days 1-5, the heating temperature of the induction high temperature furnace crucible is 700 ℃;
on day 6, the heating temperature of the induction furnace crucible is increased from 700 ℃ to 750 ℃;
the heating temperature of the induction high-temperature furnace crucible is 750 ℃ in 7-10 days;
on day 11, the heating temperature of the induction furnace crucible is increased from 750 ℃ to 800 ℃;
on the 12 th to 15 th days, the heating temperature of the induction high temperature furnace crucible is 800 ℃;
on day 16, the heating temperature of the induction furnace crucible was increased from 800 ℃ to 850 ℃;
on days 17-19, the heating temperature of the induction high temperature furnace crucible is 850 ℃;
on day 20, the heating temperature of the induction furnace crucible is increased from 850 ℃ to 900 ℃;
on day 21, the induction furnace crucible was heated to 900 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311730833.9A CN117831826A (en) | 2023-12-15 | 2023-12-15 | Ca ion generation method suitable for ECR ion source device |
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| CN202311730833.9A CN117831826A (en) | 2023-12-15 | 2023-12-15 | Ca ion generation method suitable for ECR ion source device |
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| CN117831826A true CN117831826A (en) | 2024-04-05 |
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| CN202311730833.9A Pending CN117831826A (en) | 2023-12-15 | 2023-12-15 | Ca ion generation method suitable for ECR ion source device |
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- 2023-12-15 CN CN202311730833.9A patent/CN117831826A/en active Pending
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