CN104021830B - The polynary nano-micron compound crystal radiation protection material of the banded template two dimension of a kind of inorfil - Google Patents

The polynary nano-micron compound crystal radiation protection material of the banded template two dimension of a kind of inorfil Download PDF

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Publication number
CN104021830B
CN104021830B CN201410226476.7A CN201410226476A CN104021830B CN 104021830 B CN104021830 B CN 104021830B CN 201410226476 A CN201410226476 A CN 201410226476A CN 104021830 B CN104021830 B CN 104021830B
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polynary
dimension
nano
crystal
radiation protection
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CN104021830A (en
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何洪林
董学斌
史晓亮
董胜其
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Wuhan Shengqi Radiation Protection Material Co ltd
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Wuhan Shengqi Radiation Protection Material Co ltd
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Abstract

Relate to the radiation protection material of the polynary nano-micron compound crystal of the banded template two dimension of a kind of inorganic light weight fiber. Its raw materials comprises containing Mo, containing boron material and contenting carbon material; Prepare by the following method: raw material is placed in crystal synthetic furnace, to contain Mo as synthetic furnace heater, under protective gas atmosphere, be warming up to 150 DEG C-1200 DEG C, temperature retention time 1-10h, can obtain the polynary nano-micron compound crystal of inorganic two dimension radiation protection material; In preparation process, molybdenum powder or molybdenum oxide powder water or alcohol are adjusted to pasty state, before intensification, are painted on crystal synthetic furnace heater surface. Composite crystal proportion is less than 5.0g/cm3,Length dimension can be crossed centimetre, the wide grade that reaches, and bed thickness is for receiving a micron Grade; The polynary composite crystal of two dimension comprises molybdenum, carbon, boron; Unleaded, nontoxic, non-environmental-pollution composition; And neutrons in nuclei radiation ray, electromagenetic wave radiation and x light radiation are had to absorption, decay and shielding properties.

Description

The polynary nano-micron compound crystal radiation protection material of the banded template two dimension of a kind of inorfil
Technical field
The invention belongs to materials science field, be specifically related to the polynary micron of receiving of the banded template two dimension of a kind of inorganic light weight fiber and answerThe radiation protection material of synthetic body.
Background technology
People are in the urgent need to a kind of low-gravity, high-performance, multi-functional, use safety, and decay easily high-energy ray and shielding are penetratedLinear radiation protection material that can be good.
Monodimension nanometer material is inhaled with its little diameter, large draw ratio, high anisotropy, unusual structure and peculiar performanceHaving drawn the great interest of Chinese scholars, may become the basic material of Future Information, energy field, is international material researchDisciplinary Frontiers. At present, studying more monodimension nanometer material is mainly carbon, Ge silicon, Ge ZnO, Ge CdS etc., wherein nanometerCarbon pipe is the most noticeable. In addition, researcher is exploring technology of preparing and the performance of new monodimension nanometer material in the worldFeature.
Summary of the invention
The object of the invention be to provide a kind of crystal morphology size larger, to the barrier propterty of radiation is better and preparation method is simple and easy,Comprise molybdenum, carbon, the polynary nano-micron compound crystal radiation protection material of boron two dimension and preparation method thereof.
The polynary nano-micron compound crystal of a kind of inorganic two dimension radiation protection material, its raw materials comprises containing Mo, containing boron materialAnd contenting carbon material; Prepare by the following method:
Raw material is placed in the synthetic burner hearth of crystal, to contain Mo as crystal synthetic furnace heater, under protective gas atmosphere, heats upTo 150 DEG C of-1200 DEG C of temperature retention time 1-10h, can obtain the polynary nano-micron compound crystal of inorganic two dimension radiation protection material.
Press such scheme, the polynary nano-micron compound crystal of described two dimension is the polynary nano-micron compound crystalline substance of two dimension that comprises molybdenum, carbon, boronBody.
Press such scheme, described is any one or group arbitrarily of molybdenum powder, molybdenum filament, molybdenum bar, molybdenum sheet, molybdenum oxide powder containing MoClose.
Press such scheme, in preparation process, molybdenum powder or molybdenum oxide powder water or alcohol are adjusted to pasty state, before intensification, be painted on crystal syntheticStove heater surface.
Press such scheme, described is boron powder, boric acid or boron oxide containing boron material; And described boracic material usage is less than containing Mo40wt%.
Press such scheme, described is borine containing boron material, and its consumption is less than 10% of shield gas flow rate.
Press such scheme, described contenting carbon material is any one or any combination of active carbon, graphite, CNT, coal;Described contenting carbon material consumption is less than the 40wt% containing Mo.
Press such scheme, described contenting carbon material is carbonaceous gas; Described general carbonaceous gas comprise carbon monoxide, carbon dioxide,Methane or propane; Its consumption is less than 40% of shield gas flow rate.
Press such scheme, described protective gas is hydrogen, nitrogen, argon gas or ammonia.
Beneficial effect of the present invention:
Radiation protection material provided by the invention, proportion is less than 5.0g/cm3, length of material size can be crossed Centimeter Level, and width dimensions canReach grade, bed thickness is of a size of receives a micron Grade; For comprising molybdenum, carbon, the polynary composite crystal of boron one dimension. And material is unleaded, nontoxic,Non-environmental-pollution composition;
Experimental results show that the polynary nano-micron compound crystal of inorganic two dimension provided by the invention radiation protection material to neutrons in nuclei radiation ray,Electromagenetic wave radiation and x light radiation have absorption, decay and shielding properties;
Experimental results show that the present invention itself also tool have energy gap, it is made after the thin slice of similar Graphene, both supported at a high speed fortune of electronicsMoving, its characteristic of semiconductor is applicable to again manufacturing sub-device application. Also possess higher storage lithium ability simultaneously, be expected at storage lithium electronic materialApplication aspect plays a role.
Brief description of the drawings
Fig. 1: embodiment 1 products obtained therefrom scanning electron microscope (SEM) photograph;
Fig. 2: embodiment 2 products obtained therefrom scanning electron microscope (SEM) photographs.
Detailed description of the invention
Following examples are for further illustrating technical scheme of the present invention, but not as limiting the scope of the invention.
The polynary nano-micron compound crystal of the inorganic two dimension of the present invention radiation protection material, its raw materials is for containing Mo, containing boron materialAnd contenting carbon material;
Preparation process: raw material is placed in the synthetic burner hearth of crystal, to contain Mo as crystal synthetic furnace heater, at protective gasUnder atmosphere, be warming up to 150 DEG C of-1200 DEG C of temperature retention time 1-10h, can grow the radiation of the polynary nano-micron compound crystal of inorganic two dimensionProtective materials.
The polynary nano-micron compound crystal of inorganic two dimension radiation protection material prepared by the present invention is that the two dimension that comprises molybdenum, carbon, boron is polynaryNano-micron compound crystal. , proportion is less than 5.0g/cm3, length of material size can be crossed Centimeter Level, and width dimensions can reach grade, layerThick being of a size of received a micron Grade; And material is unleaded, nontoxic, non-environmental-pollution composition.
Selected containing Mo can be molybdenum powder, molybdenum filament, molybdenum bar, molybdenum sheet, molybdenum oxide powder any one or be combined.
During as heater, preferably molybdenum filament, molybdenum bar or molybdenum sheet. Importantly, in preparation process, by molybdenum powder or molybdenum oxide powder waterOr alcohol is adjusted to pasty state, before intensification, be painted on crystal synthetic furnace heater surface.
Selected is boron powder, boric acid or boron oxide containing boron material; And boracic material usage is less than the 40wt% containing Mo.
Can also be borine containing boron material, when use and protective gas together pass into burner hearth, its consumption is less than shield gas flow rate10%。
Selected contenting carbon material can be any one or any combination of active carbon, graphite, CNT, coal. Contenting carbon materialConsumption is less than the 40wt% containing Mo.
Selected contenting carbon material can also be carbonaceous gas; Carbonaceous gas comprises carbon monoxide, carbon dioxide, methane or propane; MakeUsed time and protective gas together pass into burner hearth, and its consumption is less than 40% of shield gas flow rate.
Selected protective gas is hydrogen, nitrogen, argon gas or ammonia.
Experimental results show that the polynary nano-micron compound crystal of inorganic two dimension provided by the invention radiation protection material to neutrons in nuclei radiation ray,Electromagenetic wave radiation and x radiation have absorption, decay and shielding properties.
Embodiment 1
1) metal molybdenum filament is washed the dry synthetic burner hearth inner surface of high temperature crystal that is placed in of PROCESS FOR TREATMENT through the conventional Chilly such as acid and alkali; Do with molybdenum filamentFor the synthetic burner hearth internal heat generation body of crystal uses, metal molybdenum powder particle is adjusted to pasty state with alcohol agent and is painted on heater surface; Meanwhile, addEnter the boric acid and the active carbon that respectively account for Mo weight 40wt% in synthetic furnace chamber;
2) hydrogen is protective gas, passes in high temperature crystal synthetic furnace by security regulations, and high temperature crystal synthetic furnace gas flow is for justPress;
3) energising heating, being warming up to 150 DEG C of temperature retention times is 2h, is cooled to 130 DEG C of taking-ups in power-off stove, obtains inorganic two dimensionPolynary nano-micron compound crystal radiation protection material.
The present embodiment protection composite X ray detects, according to the mensuration of GBZ/147X radiation protection composite fade performanceStandard, adopts protection level X ray reference radiation PTWUNIDOS dosemeter, and test condition 40KV-80KV/4MMAI, surveysTest result is 140. The present embodiment scanning electron microscope (SEM) photograph is with reference to accompanying drawing 1.
Experiment also prove the polynary nano-micron compound crystal of inorganic two dimension provided by the invention radiation protection material to neutrons in nuclei radiation penetrateLine, electromagenetic wave radiation have absorption, decay and shielding properties.
Embodiment 2
1) metal molybdenum bar washes through the conventional Chilly such as acid and alkali that PROCESS FOR TREATMENT is dry to be placed in the synthetic burner hearth of high temperature crystal; Using molybdenum sheet as crystalline substanceThe synthetic burner hearth internal heat generation body of body uses, and molybdenum oxide powder particle water is adjusted to pasty state and is painted on heater surface; Meanwhile, add respectively and account forBorax and the active carbon of Mo weight 30wt% in heat size device;
2) nitrogen is that protective gas passes in high temperature crystal synthetic furnace by security regulations, and high temperature crystal synthetic furnace gas flow is malleation;
3) energising heating, being warming up to 270 DEG C of temperature retention times is 10h, is cooled to 130 DEG C of taking-ups in power-off stove, obtains inorganic twoTie up polynary nano-micron compound crystal radiation protection material.
The present embodiment protection composite X ray detects, according to the mensuration of GBZ/147X radiation protection composite fade performanceStandard, adopts protection level X ray reference radiation PTWUNIDOS dosemeter, and test condition 40KV-80KV/4MMAI, surveysTest result is 200. The present embodiment scanning electron microscope (SEM) photograph is with reference to accompanying drawing 2.
Experiment also prove the polynary nano-micron compound crystal of inorganic two dimension provided by the invention radiation protection material to neutrons in nuclei radiation penetrateLine, electromagenetic wave radiation have absorption, decay and shielding properties.
Embodiment 3
1) metal molybdenum sheet washes through the conventional Chilly such as acid and alkali that PROCESS FOR TREATMENT is dry to be placed in the synthetic burner hearth of high temperature crystal; Using molybdenum bar as crystalline substanceThe synthetic burner hearth internal heat generation body of body uses, and molybdenum oxide powder particle water is adjusted to pasty state and is painted on heater surface; Meanwhile, add respectively and account forBoron powder and the active carbon of Mo weight 20wt% in heat size device;
2) nitrogen is that protective gas passes in high temperature crystal synthetic furnace by security regulations, and high temperature crystal synthetic furnace gas flow is malleation;
3) energising heating, being warming up to 400 DEG C of temperature retention times is 6h, is cooled to 130 DEG C of taking-ups in power-off stove, obtains inorganic two dimensionPolynary nano-micron compound crystal radiation protection material.
The present embodiment protection composite X ray detects, according to the mensuration of GBZ/147X radiation protection composite fade performanceStandard, adopts protection level X ray reference radiation PTWUNIDOS dosemeter, and test condition 40KV-80KV/4MMAI, surveysTest result is 300.
Experiment also prove the polynary nano-micron compound crystal of inorganic two dimension provided by the invention radiation protection material to neutrons in nuclei radiation penetrateLine, electromagenetic wave radiation have absorption, decay and shielding properties.
Embodiment 4
1) metal molybdenum sheet is washed the dry high temperature crystal synthetic furnace that is placed in of PROCESS FOR TREATMENT through the conventional Chilly such as acid and alkali; Close as crystal using molybdenum filamentBecome burner hearth internal heat generation body to use, molybdenum oxide powder particle water is adjusted to pasty state and is painted on heater surface; Meanwhile, between the stage of reaction, pass intoAccount for the borane gases of nitrogen protection gas flow 10%, pass into the methane gas that accounts for nitrogen protection gas flow 10% in reacting furnace;
2) nitrogen is that protective gas passes in high temperature crystal synthetic furnace by security regulations, and high temperature crystal synthetic furnace gas flow is malleation;
3) energising heating, being warming up to 500 DEG C of temperature retention times is 6h, is cooled to 130 DEG C of taking-ups in power-off stove, obtains inorganic two dimensionPolynary nano-micron compound crystal radiation protection material.
The present embodiment protection composite X ray detects, according to the mensuration of GBZ/147X radiation protection composite fade performanceStandard, adopts protection level X ray reference radiation PTWUNIDOS dosemeter, and test condition 40KV-80KV/4MMAI, surveysTest result is 350.
Experiment also prove the polynary nano-micron compound crystal of inorganic two dimension provided by the invention radiation protection material to neutrons in nuclei radiation penetrateLine, electromagenetic wave radiation have absorption, decay and shielding properties.
Embodiment 5
1) metal molybdenum bar is washed the dry high temperature crystal synthetic furnace that is placed in of PROCESS FOR TREATMENT through the conventional Chilly such as acid and alkali; Close as crystal using molybdenum barBecome burner hearth internal heat generation body to use, molybdenum oxide powder particle water is adjusted to pasty state and is painted on heater surface; Meanwhile, add and account for heat size deviceThe borax of interior Mo weight 40wt%; Between the stage of reaction, pass into the methane gas that accounts for argon shield gas flow 25% in reacting furnace;
2) argon gas is that protective gas passes in high temperature crystal synthetic furnace by security regulations, and flow is malleation;
3) energising heating, being warming up to 500 DEG C of temperature retention times is 6h, is cooled to 130 DEG C of taking-ups in power-off stove, obtains inorganic two dimensionPolynary nano-micron compound crystal radiation protection material.
The present embodiment protection composite X ray detects, according to the mensuration of GBZ/147X radiation protection composite fade performanceStandard, adopts protection level X ray reference radiation PTWUNIDOS dosemeter, and test condition 40KV-80KV/4MMAI, surveysTest result is 500.
Experiment also prove the polynary nano-micron compound crystal of inorganic two dimension provided by the invention radiation protection material to neutrons in nuclei radiation penetrateLine, electromagenetic wave radiation have absorption, decay and shielding properties.
Embodiment 6
1) metal molybdenum bar washes through the conventional Chilly such as acid and alkali that PROCESS FOR TREATMENT is dry to be placed in the synthetic burner hearth of high temperature crystal; Using molybdenum sheet as crystalline substanceThe synthetic burner hearth internal heat generation body of body uses, and molybdenum oxide powder particle water is adjusted to pasty state and is painted on heater surface; Meanwhile, add and account for stoveThe borax of Mo weight 5wt% in container; Between the stage of reaction, pass into the methane gas that accounts for argon shield gas flow 25% in reacting furnaceBody;
2) argon gas is that protective gas passes in high temperature crystal synthetic furnace by security regulations, and flow is malleation;
3) energising heating, being warming up to 650 DEG C of temperature retention times is 2h, is cooled to 130 DEG C of taking-ups in power-off stove, obtains inorganic two dimensionPolynary nano-micron compound crystal radiation protection material.
The present embodiment protection composite X ray detects, according to the mensuration of GBZ/147X radiation protection composite fade performanceStandard, adopts protection level X ray reference radiation PTWUNIDOS dosemeter, and test condition 40KV-80KV/4MMAI, surveysTest result is 550.
Experiment also prove the polynary nano-micron compound crystal of inorganic two dimension provided by the invention radiation protection material to neutrons in nuclei radiation penetrateLine, electromagenetic wave radiation have absorption, decay and shielding properties.
Embodiment 7
1) metal molybdenum bar washes through the conventional Chilly such as acid and alkali that PROCESS FOR TREATMENT is dry to be placed in the synthetic burner hearth of high temperature crystal; Using molybdenum bar as crystalline substanceThe synthetic burner hearth internal heat generation body of body uses, and molybdenum oxide powder particle water is adjusted to pasty state and is painted on heater surface; Meanwhile, add and account for stoveThe borax of Mo weight 1wt% in container; Between the stage of reaction, pass into an oxidation that accounts for argon shield gas flow 30% in reacting furnaceCarbon gas;
2) argon gas is that protective gas passes in high temperature crystal synthetic furnace by security regulations, and flow is malleation;
3) energising heating, being warming up to 800 DEG C of temperature retention times is 1h, is cooled to 130 DEG C of taking-ups in power-off stove, obtains inorganic two dimensionPolynary nano-micron compound crystal radiation protection material.
The present embodiment protection composite X ray detects, according to the mensuration of GBZ/147X radiation protection composite fade performanceStandard, adopts protection level X ray reference radiation PTWUNIDOS dosemeter, and test condition 40KV-80KV/4MMAI, surveysTest result is 600.
Experiment also prove the polynary nano-micron compound crystal of inorganic two dimension provided by the invention radiation protection material to neutrons in nuclei radiation penetrateLine, electromagenetic wave radiation have absorption, decay and shielding properties.
Embodiment 8
1) metal molybdenum sheet washes through the conventional Chilly such as acid and alkali that PROCESS FOR TREATMENT is dry to be placed in the synthetic furnace chamber of high temperature crystal; Using molybdenum bar as crystalline substanceThe synthetic burner hearth internal heat generation body of body uses, and molybdenum oxide powder particle water is adjusted to pasty state and is painted on synthetic furnace chamber internal heat generation surface; Meanwhile,Add the borax that accounts for Mo weight 35wt% in heat size device; Between the stage of reaction, pass into and in reacting furnace, account for argon shield gas flow 40%Carbon dioxide;
2) ammonia is that protective gas passes in high temperature crystal synthetic furnace by security regulations, and flow is malleation;
3) energising heating, being warming up to 1000 DEG C of temperature retention times is 1h, is cooled to 130 DEG C of taking-ups in power-off stove, obtains inorganic twoTie up polynary nano-micron compound crystal radiation protection material.
The present embodiment protection composite X ray detects, according to the mensuration of GBZ/147X radiation protection composite fade performanceStandard, adopts protection level X ray reference radiation PTWUNIDOS dosemeter, test condition 40KV-80KV/4MMAI,Test result is 633.
Experiment also prove the polynary nano-micron compound crystal of inorganic two dimension provided by the invention radiation protection material to neutrons in nuclei radiation penetrateLine, electromagenetic wave radiation have absorption, decay and shielding properties.
Embodiment 9
1) metal molybdenum sheet washes through the conventional Chilly such as acid and alkali that PROCESS FOR TREATMENT is dry to be placed in the synthetic furnace chamber of high temperature crystal; Using molybdenum bar as crystalline substanceThe synthetic burner hearth internal heat generation body of body uses, and molybdenum oxide powder particle water is adjusted to pasty state and is painted on heater surface; Meanwhile, add and account for stoveThe boron oxide of Mo weight 40wt% in container; Between the stage of reaction, pass into the dioxy that accounts for protection of ammonia gas flow 27% in reacting furnaceChange carbon gas;
2) ammonia is that protective gas passes in high temperature crystal synthetic furnace by security regulations, and flow is malleation;
3) energising heating, being warming up to 1200 DEG C of temperature retention times is 1h, is cooled to 130 DEG C of taking-ups in power-off stove, obtains inorganic receivingMicron composite crystal radiation protection material.
The present embodiment protection composite X ray detects, according to the mensuration of GBZ/147X radiation protection composite fade performanceStandard, adopts protection level X ray reference radiation PTWUNIDOS dosemeter, and test condition 40KV-80KV/4MMAI, surveysTest result is 455.
Experiment also prove the polynary nano-micron compound crystal of inorganic two dimension provided by the invention radiation protection material to neutrons in nuclei radiation penetrateLine, electromagenetic wave radiation have absorption, decay and shielding properties.

Claims (6)

1. the polynary nano-micron compound crystal of an inorganic two dimension radiation protection material, it is characterized in that raw materials comprise containing Mo,Containing boron material and contenting carbon material; Prepare by the following method:
Raw material is placed in the synthetic burner hearth of crystal, to contain Mo as crystal synthetic furnace heater, under protective gas atmosphere, heats upTo 150 DEG C of-1200 DEG C of temperature retention time 1-10h, can obtain the polynary nano-micron compound crystal of inorganic two dimension radiation protection material.
2. the polynary nano-micron compound crystal of inorganic two dimension as claimed in claim 1 radiation protection material, contains described in it is characterized in thatMo is any one or any combination of molybdenum powder, molybdenum filament, molybdenum bar, molybdenum sheet, molybdenum oxide powder.
3. the polynary nano-micron compound crystal of inorganic two dimension as claimed in claim 1 radiation protection material, contains described in it is characterized in thatBoron material is boron powder, boric acid or boron oxide; And described boracic material usage is less than the 40wt% containing Mo.
4. the polynary nano-micron compound crystal of inorganic two dimension as claimed in claim 1 radiation protection material, contains described in it is characterized in thatBoron material is borine, and its consumption is less than 10% of shield gas flow rate.
5. the polynary nano-micron compound crystal of inorganic two dimension as claimed in claim 1 radiation protection material, contains described in it is characterized in thatCarbon Materials is any one or any combination of active carbon, graphite, CNT, coal; Described contenting carbon material consumption is less than and containsThe 40wt% of Mo.
6. the polynary nano-micron compound crystal of inorganic two dimension as claimed in claim 1 radiation protection material, is characterized in that described guarantorProtecting gas is hydrogen, nitrogen, argon gas or ammonia.
CN201410226476.7A 2014-05-26 2014-05-26 The polynary nano-micron compound crystal radiation protection material of the banded template two dimension of a kind of inorfil Expired - Fee Related CN104021830B (en)

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Citations (3)

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CN1199746A (en) * 1997-05-19 1998-11-25 周胜刚 Colloid boron polymer with protection function and its preparation, product and use
US20030010939A1 (en) * 1998-12-07 2003-01-16 Meridian Research And Development Lightweight radiation protective articles and methods for making them
CN101198442A (en) * 2005-07-22 2008-06-11 Tdy工业公司 Composite materials

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JP2003227896A (en) * 2002-02-01 2003-08-15 Mitsubishi Heavy Ind Ltd Radiation shield

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN1199746A (en) * 1997-05-19 1998-11-25 周胜刚 Colloid boron polymer with protection function and its preparation, product and use
US20030010939A1 (en) * 1998-12-07 2003-01-16 Meridian Research And Development Lightweight radiation protective articles and methods for making them
CN101198442A (en) * 2005-07-22 2008-06-11 Tdy工业公司 Composite materials

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