CN109852927A - A kind of membrane structure for the boron-rich coating of Boron-coated neutron detector - Google Patents
A kind of membrane structure for the boron-rich coating of Boron-coated neutron detector Download PDFInfo
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- CN109852927A CN109852927A CN201910180279.9A CN201910180279A CN109852927A CN 109852927 A CN109852927 A CN 109852927A CN 201910180279 A CN201910180279 A CN 201910180279A CN 109852927 A CN109852927 A CN 109852927A
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Abstract
The present invention relates to a kind of membrane structures for the boron-rich coating of Boron-coated neutron detector, including substrate and B4C film is it is characterized in that, the substrate and B4Metal layer is provided between C film;The material of the metal layer is active metal;The active metal is preferably one of Ti, Ni, Al, Mg or MgAl alloy;The thickness of the metal layer is less than 100nm.Compared with prior art, the present invention greatly strengthens B4Adhesion effect between C film and aluminium substrate;Solve B4The problem of C film falls off from aluminium substrate has preparation simple, and film structure is simple, technical maturity, can preparative it is strong the advantages that.
Description
Technical field
The present invention relates to field of film preparation, are related to a kind of Boron-coated neutron detector, more particularly, to one kind for applying boron
The membrane structure of the boron-rich coating of neutron detector.
Background technique
Common neutron detector is 3He neutron detector, but the inventory of 3He gas is increasingly reduced, both at home and abroad gradually
Start to research and develop Boron-coated neutron detector.For the Boron-coated neutron detector under neutron beam that works, substrate is aluminium substrate, in base
The coating that bottom surface and neutron react is boron-rich coating, which is made of B4C film.When neutron enters B4C film, meeting
And B410B in C reacts and is converted into α particle.α particle enters and ionizes the work gas in Boron-coated neutron detector
Avalanche effect occurs for the electronics of body, generation, and detector begins with the output of charge signal.
So far, the structure of Boron-coated neutron detector is all to be coated with the B of single layer in aluminium base bottom surface4C film.In order to obtain
Obtain maximum neutron detection efficiency, B4The thickness of C film is usually 1 μm~2 μm.Because of the B of 1 μm~2 μ m-thicks4C film, which exists, answers
The big problem of power, while the roughness of aluminium substrate is also bigger than normal and surface is covered with oxide layer, so be coated on aluminum substrates
B4Adhesive force between C film and substrate is smaller, there are problems that falling off from substrate, how to overcome the problems, such as that this is that research and development apply boron
One of the difficult point for needing to overcome during neutron detector.
In existing research, technique and up to 16kW that only Carina Hglund et al. has used substrate to heat
Target rifle power, is successfully prepared 1 μm or more of B on aluminum substrates4C film.Requirement of this method to magnetron sputtering apparatus structure
It is very high, prepare B4The cost of C film is also very high.In practical applications, there is an urgent need to a kind of novel, adhesion effect it is strong and property
Valence is than the higher membrane structure for the boron-rich coating of Boron-coated neutron detector.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind for applying boron neutron
The membrane structure of the boron-rich coating of detector.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of membrane structure for the boron-rich coating of Boron-coated neutron detector, including substrate and B4C film it is characterized in that,
The substrate and B4Metal layer is provided between C film.
The material of the metal layer is active metal.
The Gibbs free energy of active metal described in the active metal is no more than the Gibbs free energy of Al metal;It is excellent
It is selected as Ti, Ni, Al, Mg or MgAl alloy.
Active metal in the present invention should be in normal temperature condition or under conditions of close to room temperature, can be from Al2O3In it is more
Acquisition O element, therefore should select Gibbs free energy be close to or smaller than Al material.
The thickness of the metal layer is less than 100nm, preferably 15nm.
The B4The preparation process of C film and metal layer is magnetron sputtering.
Inert gas in the magnetron sputtering process is the Ar gas that purity is 99.99%, sputters B4Sputtering gas when C target
Pressure is 10-12mtorr, and sputtering pressure when splash-proofing sputtering metal target is 1.0-2.0mtorr.
Main operating parameters in the magnetron sputtering process are as follows: base vacuum is better than 3.0 × 10-4Pa;B4C target and metal
The range (substrate is at a distance from target) of target is 6.0cm;B4The sputtering power of C target is 100W, and the sputtering power of metallic target is
40W。
The material of the substrate is aluminium.
The B4C film with a thickness of 1 μm~2 μm.
The operation principle of the present invention is that: the present invention is in aluminum substrate and B4Metal layer is added between C as adhesive layer, metal
Layer is active metal, and active metal is easy and other atoms with oxidisability form the oxidation on chemical bond, such as basal layer
B in object or boron carbide+, therefore between aluminum substrate and active metal and B4Pass through chemical bonds between C and active metal,
Increase adhesion effect between layers.
Compared with prior art, invention has the advantages that
(1) present invention traditional boron-rich coated film structure [aluminum substrate | B4C] in increase one layer of certain thickness gold
Category layer, and formation new thin film structure [aluminum substrate | metal layer | B4C], the thickness by adjusting metal layer can make B4C film with
Adhesion effect between aluminium substrate substantially enhances, to solve B4The problem of C film falls off from aluminium substrate;Metal layer thickness is necessary
Moderate, if thicknesses of layers is too small, film layer is discontinuous, may cause the B of regional area4C film separation;If thicknesses of layers mistake
Greatly, since the grain growth of metallic diaphragm is perfect, interatomic force increases, and B element and the combination effect of O element are deteriorated,
Adhesiveness is caused to reduce.
(2) present invention is being coated with B4The Ar gas sputtering pressure that 10mTorr~12mTorr has been used when C film, can obtain
More loose metal layer and B4C film.Metal layer can more effectively with the oxide layer and B in aluminium substrate4C film occurs anti-
It answers, to obtain bigger diffusion region, further enhances B4Adhesion effect between C film and aluminium substrate.B4The stress of C film is more
It is small, it avoids falling off from aluminium substrate since stress is larger;The present invention is when being coated with metal layer, using 1.0-2.0mtorr's
Ar gas sputtering pressure, to promote energy when metallic atom is incident on aluminium substrate, to improve between metal layer thin film and aluminium substrate
Adhesion effect, the sputtering pressure of magnetron sputtering is carried out preferably, to solve B jointly4The problem of C film falls off from aluminium substrate.
(3) the boron-rich coating of Boron-coated neutron detector of the present invention membrane structure [aluminum substrate | metal layer | B4C] to magnetic control
The requirement of sputtering equipment is lower, and preparation is simple, and film structure is simple, technical maturity, can preparative it is strong.
Detailed description of the invention
Fig. 1 is structural representation of the invention;
Fig. 2 is B of the present invention4C membrane stress value and sputtering B4The relational graph of sputtering pressure when C;
In Fig. 1,1 is substrate, and 2 be B4C film, 3 be metal layer.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1
A kind of membrane structure for the boron-rich coating of Boron-coated neutron detector, as shown in Figure 1, including substrate 1 and B4C film
2, substrate 1 and B4Certain thickness metal layer 3 is provided between C film 2.The aluminium model AA1060 of substrate 1;B4The thickness of C film
Degree is 1.2 μm;The material of metal layer 3 is active metal, and the Gibbs free energy of active metal described in the active metal is no more than
The Gibbs free energy of Al metal can be from Al in normal temperature condition or under conditions of close to room temperature2O3In more obtain O member
Element, the material of metal layer 3 is MgAl alloy in the present embodiment, with a thickness of 15nm.
Metal layer 3 and B4The preparation process of C film 2 is all made of magnetron sputtering.In the present embodiment, metal layer 3 and B are prepared4C
Sputter gas when film 2 is pure Ar gas, is coated with B4Sputtering pressure when C film 2 is 10mTorr, can be obtained loose
B4C film 2 reduces B4Stress inside C film 2;And sputtering pressure when being coated with MgAl is 1mtorr, to promote metallic atom
It is incident on energy when aluminium substrate, to improve the adhesion effect between MgAl alloy firm and aluminium substrate, solves B jointly4C film
The problem of falling off from aluminium substrate.Base vacuum is better than 3.0 × 10 in magnetron sputtering process-4Pa;Range is 6.0cm;B4C target
Sputtering power be 100W, the sputtering power of metallic target is 40W.
Pure Ar gas effects of air pressure B in magnetron sputtering process4C membrane stress, as shown in Fig. 2, as seen from the figure, when being coated with B4C is thin
Ar gas air pressure when film is higher, B4The stress of C film is smaller;When being coated with B4When Ar gas air pressure when C film is higher than 8.0mTorr,
B4The stress of C film tends towards stability.
Embodiment 2
A kind of membrane structure for the boron-rich coating of Boron-coated neutron detector, as shown in Figure 1, including substrate 1 and B4C film
2, substrate 1 and B4Certain thickness metal layer 3 is provided between C film 2.The aluminium model AA1060 of substrate 1.B4The thickness of C film
Degree is 1 μm.The material of metal layer 3 is active metal, and the Gibbs free energy of active metal described in the active metal is no more than Al
The Gibbs free energy of metal can be from Al in normal temperature condition or under conditions of close to room temperature2O3In more obtain O member
Element, the material of metal layer 3 is MgAl alloy in the present embodiment, with a thickness of 100nm.
Metal layer 3 and B4The preparation process of C film 2 is all made of magnetron sputtering.In the present embodiment, metal layer 3 and B are prepared4C
Sputter gas when film 2 is pure Ar gas, is coated with B4Sputtering pressure when C film 2 is 12mTorr, can be obtained loose
B4C film 2 reduces B4Stress inside C film 2;And sputtering pressure when being coated with MgAl is 1mtorr, to promote metallic atom
It is incident on energy when aluminium substrate, to improve the adhesion effect between MgAl alloy firm and aluminium substrate, solves B jointly4C film
The problem of falling off from aluminium substrate.Base vacuum is better than 3.0 × 10 in magnetron sputtering process-4Pa;Range is 6.0cm;B4C target
Sputtering power be 100W, the sputtering power of metallic target is 40W.
Embodiment 3
A kind of membrane structure for the boron-rich coating of Boron-coated neutron detector, as shown in Figure 1, including substrate 1 and B4C film
2, substrate 1 and B4Certain thickness metal layer 3 is provided between C film 2.The aluminium model AA1060 of substrate 1.B4The thickness of C film
Degree is 2 μm.The material of metal layer 3 is active metal, and the Gibbs free energy of active metal described in the active metal is no more than Al
The Gibbs free energy of metal can be from Al in normal temperature condition or under conditions of close to room temperature2O3In more obtain O member
Element, the material of metal layer 3 is MgAl alloy in the present embodiment, with a thickness of 50nm.
Metal layer 3 and B4The preparation process of C film 2 is all made of magnetron sputtering.In the present embodiment, metal layer 3 and B are prepared4C
Sputter gas when film 2 is pure Ar gas, is coated with B4Sputtering pressure when C film 2 is 11mTorr, can be obtained loose
B4C film 2 reduces B4Stress inside C film 2;And sputtering pressure when being coated with MgAl is 1mtorr, to promote metallic atom
It is incident on energy when aluminium substrate, to improve the adhesion effect between MgAl alloy firm and aluminium substrate, solves B jointly4C film
The problem of falling off from aluminium substrate.Base vacuum is better than 3.0 × 10 in magnetron sputtering process-4Pa;Range is 6.0cm;B4C target
Sputtering power be 100W, the sputtering power of metallic target is 40W.
Embodiment 4
A kind of membrane structure for the boron-rich coating of Boron-coated neutron detector, as shown in Figure 1, including substrate 1 and B4C film
2, substrate 1 and B4Certain thickness metal layer 3 is provided between C film 2.The aluminium model AA1060 of substrate 1.B4The thickness of C film
Degree is 2 μm.The material of metal layer 3 is active metal, and the Gibbs free energy of active metal described in the active metal is no more than Al
The Gibbs free energy of metal can be from Al in normal temperature condition or under conditions of close to room temperature2O3In more obtain O member
Element, the material of metal layer 3 is Ti in the present embodiment, with a thickness of 15nm.
Metal layer 3 and B4The preparation process of C film 2 is all made of magnetron sputtering.In the present embodiment, metal layer 3 and B are prepared4C
Sputter gas when film 2 is pure Ar gas, is coated with B4Sputtering pressure when C film 2 is 11mTorr, can be obtained loose
B4C film 2 reduces B4Stress inside C film 2;And sputtering pressure when being coated with Ti metal layer is 2mtorr, to promote metal
Atom is incident on energy when aluminium substrate, to improve the adhesion effect between Ti metal layer and aluminium substrate, solves B jointly4C film
The problem of falling off from aluminium substrate.Base vacuum is better than 3.0 × 10 in magnetron sputtering process-4Pa;Range is 6.0cm;B4C target
Sputtering power be 100W, the sputtering power of metallic target is 40W.
Embodiment 5
A kind of membrane structure for the boron-rich coating of Boron-coated neutron detector, as shown in Figure 1, including substrate 1 and B4C film
2, substrate 1 and B4Certain thickness metal layer 3 is provided between C film 2.The aluminium model AA1060 of substrate 1.B4The thickness of C film
Degree is 2 μm.The material of metal layer 3 is active metal, and the Gibbs free energy of active metal described in the active metal is no more than Al
The Gibbs free energy of metal can be from Al in normal temperature condition or under conditions of close to room temperature2O3In more obtain O member
Element, the material of metal layer 3 is Ni in the present embodiment, with a thickness of 15nm.
Metal layer 3 and B4The preparation process of C film 2 is all made of magnetron sputtering.In the present embodiment, metal layer 3 and B are prepared4C
Sputter gas when film 2 is pure Ar gas, is coated with B4Sputtering pressure when C film 2 is 11mTorr, can be obtained loose
B4C film 2 reduces B4Stress inside C film 2;And sputtering pressure when being coated with Ni metal layer is 2mtorr, to promote metal
Atom is incident on energy when aluminium substrate, to improve the adhesion effect between Ni metal layer and aluminium substrate, solves B jointly4C film
The problem of falling off from aluminium substrate.Base vacuum is better than 3.0 × 10 in magnetron sputtering process-4Pa;Range is 6.0cm;B4C target
Sputtering power be 100W, the sputtering power of metallic target is 40W.
Embodiment 6
A kind of membrane structure for the boron-rich coating of Boron-coated neutron detector, as shown in Figure 1, including substrate 1 and B4C film
2, substrate 1 and B4Certain thickness metal layer 3 is provided between C film 2.The aluminium model AA1060 of substrate 1.B4The thickness of C film
Degree is 2 μm.The material of metal layer 3 is active metal, and the Gibbs free energy of active metal described in the active metal is no more than Al
The Gibbs free energy of metal can be from Al in normal temperature condition or under conditions of close to room temperature2O3In more obtain O member
Element, the material of metal layer 3 is Al in the present embodiment, with a thickness of 15nm.
Metal layer 3 and B4The preparation process of C film 2 is all made of magnetron sputtering.In the present embodiment, metal layer 3 and B are prepared4C
Sputter gas when film 2 is pure Ar gas, is coated with B4Sputtering pressure when C film 2 is 11mTorr, can be obtained loose
B4C film 2 reduces B4Stress inside C film 2;And sputtering pressure when being coated with Al metal layer is 2mtorr, to promote metal
Atom is incident on energy when aluminium substrate, to improve the adhesion effect between Al metal layer and aluminium substrate, solves B jointly4C film
The problem of falling off from aluminium substrate.Base vacuum is better than 3.0 × 10 in magnetron sputtering process-4Pa;Range is 6.0cm;B4C target
Sputtering power be 100W, the sputtering power of metallic target is 40W.
Embodiment 7
A kind of membrane structure for the boron-rich coating of Boron-coated neutron detector, as shown in Figure 1, including substrate 1 and B4C film
2, substrate 1 and B4Certain thickness metal layer 3 is provided between C film 2.The aluminium model AA1060 of substrate 1.B4The thickness of C film
Degree is 2 μm.The material of metal layer 3 is active metal, and the Gibbs free energy of active metal described in the active metal is no more than Al
The Gibbs free energy of metal can be from Al in normal temperature condition or under conditions of close to room temperature2O3In more obtain O member
Element, the material of metal layer 3 is Mg in the present embodiment, with a thickness of 15nm.
Metal layer 3 and B4The preparation process of C film 2 is all made of magnetron sputtering.In the present embodiment, metal layer 3 and B are prepared4C
Sputter gas when film 2 is pure Ar gas, is coated with B4Sputtering pressure when C film 2 is 11mTorr, can be obtained loose
B4C film 2 reduces B4Stress inside C film 2;And sputtering pressure when being coated with Mg metal layer is 2mtorr, to promote metal
Atom is incident on energy when aluminium substrate, to improve the adhesion effect between Mg metal layer and aluminium substrate, solves B jointly4C film
The problem of falling off from aluminium substrate.Base vacuum is better than 3.0 × 10 in magnetron sputtering process-4Pa;Range is 6.0cm;B4C target
Sputtering power be 100W, the sputtering power of metallic target is 40W.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (10)
1. a kind of membrane structure for the boron-rich coating of Boron-coated neutron detector, including substrate (1) and B4C film (2) its feature exists
In the substrate (1) and B4Metal layer (3) are provided between C film (2).
2. a kind of membrane structure for the boron-rich coating of Boron-coated neutron detector according to claim 1, which is characterized in that
The material of the metal layer (3) is active metal.
3. a kind of membrane structure for the boron-rich coating of Boron-coated neutron detector according to claim 2, which is characterized in that
The Gibbs free energy of the active metal is no more than the Gibbs free energy of Al metal;Preferably Ti, Ni, Al, Mg or MgAl
Alloy.
4. a kind of membrane structure for the boron-rich coating of Boron-coated neutron detector according to claim 1, which is characterized in that
The thickness of the metal layer (3) is no more than 100nm.
5. a kind of membrane structure for the boron-rich coating of Boron-coated neutron detector according to claim 4, which is characterized in that
The metal layer (3) with a thickness of 15nm.
6. a kind of membrane structure for the boron-rich coating of Boron-coated neutron detector according to claim 1, which is characterized in that
The B4The preparation process of C film (2) and metal layer (3) is magnetron sputtering.
7. a kind of membrane structure for the boron-rich coating of Boron-coated neutron detector according to claim 6, which is characterized in that
Inert gas in the magnetron sputtering process is the Ar gas that purity is 99.99%, sputters B4Sputtering pressure when C target is 10-
12mtorr, sputtering pressure when splash-proofing sputtering metal target are 1.0-2.0mtorr.
8. a kind of membrane structure for the boron-rich coating of Boron-coated neutron detector according to claim 6, the magnetic control splash
During penetrating: base vacuum is better than 3.0 × 10-4Pa;B4The range of C target and metallic target is 6.0cm;B4The sputtering power of C target
For 100W, the sputtering power of metallic target is 40W.
9. a kind of membrane structure for the boron-rich coating of Boron-coated neutron detector according to claim 1, which is characterized in that
The material of the substrate (1) is aluminium.
10. a kind of membrane structure for the boron-rich coating of Boron-coated neutron detector according to claim 1, feature exist
In the B4C film (2) with a thickness of 1 μm~2 μm.
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CN114481030A (en) * | 2022-01-26 | 2022-05-13 | 苏州闻道电子科技有限公司 | Solid neutron conversion layer and preparation method and application thereof |
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