CN114106391B - Treatment method for improving local wettability of surface of GDP hollow microsphere and avoiding accelerated oxidation - Google Patents
Treatment method for improving local wettability of surface of GDP hollow microsphere and avoiding accelerated oxidation Download PDFInfo
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- CN114106391B CN114106391B CN202111419033.6A CN202111419033A CN114106391B CN 114106391 B CN114106391 B CN 114106391B CN 202111419033 A CN202111419033 A CN 202111419033A CN 114106391 B CN114106391 B CN 114106391B
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Abstract
The invention discloses a processing method for improving the local wettability of the surface of a GDP (gas diffusion plate) hollow microsphere and avoiding accelerated oxidation, which is characterized in that in the preparation process of assembling the GDP hollow microsphere and a quartz gas-filled tube, a mask assembly is adopted to shield the surface of the GDP hollow microsphere, so that a local bonding area matched with the gas-filled tube on the GDP hollow microsphere is exposed outside, and then argon plasma is adopted to process the exposed local bonding area, so that the wettability of adhesive liquid in the local bonding area is improved, and the bonding performance is further improved. The invention provides a processing method for improving the local wettability of the surface of a GDP hollow microsphere and avoiding accelerated oxidation, which is characterized in that a non-bonding area (namely an area except glue spots) is shielded in a shielding mode by a mask component, so that the shielded area of the microsphere cannot be processed during plasma processing, and cannot be irradiated by ultraviolet light in the later adhesive curing process, thereby avoiding the accelerated oxidation of the microsphere.
Description
Technical Field
The invention belongs to the field of polymer processing and forming, and particularly relates to a processing method for improving the surface local wettability of a Glow Discharge Polymer (GDP) hollow microsphere and avoiding accelerated oxidation in the surface local modification treatment of the GDP hollow microsphere.
Background
In order to solve the contradiction between the environmental destruction and the increasing global energy demand in traditional energy exploitation and utilization, advanced countries such as the united states have made continuous years of investment in Inertial Confinement Fusion (ICF) research. In the field of ICF research, glow Discharge Polymer (GDP) hollow microspheres composed of low atomic number elements C and H play an important role. On the GDP hollow microsphere with the diameter of hundreds of microns to several millimeters, a gas filling hole with the diameter of tens of microns to several microns is processed by the technology of femtosecond laser processing and the like, a quartz or glass gas filling tube is inserted into the gas filling hole, then the gap between the gas filling hole and the gas filling tube is filled by adhesive, and the gas filling hole and the gas filling tube are bonded and sealed. The fuel gas (generally deuterium or a mixture of deuterium and tritium) for ICF is injected into the GDP hollow microspheres through a gas filling tube, and then a spherical shell-shaped fuel ice layer is obtained through ultralow temperature (about 18K, namely-255 ℃) freezing. The above process has high requirements for gas tightness between the GDP hollow microsphere/gas filled tube.
In practice, chemical oxidation, electric spark, ozone oxidation, oxygen plasma and the like are often used for surface modification of nonpolar plastics such as polyethylene and polypropylene to increase their polarity. However, these methods are not suitable for surface modification of GDP hollow microspheres, mainly because these methods accelerate oxidation of GDP hollow microspheres, which may have serious adverse effects on fusion physical experiments. Even if the argon plasma treatment method without directly introducing oxygen is adopted, the GDP hollow microspheres can be oxidized by the combined action of oxygen, water and ultraviolet rays in the environment at an accelerated speed due to more 'dangling bonds' formed after treatment. At present, an effective method for improving the surface wettability of the GDP hollow microspheres to improve the bonding performance without accelerating oxidation is not found.
In addition, during the subsequent sealing and bonding process of the GDP hollow microspheres and the gas-filled tube, ultraviolet light is often used for irradiating and curing the low temperature resistant adhesive. Ultraviolet irradiation is another factor that accelerates oxidation, and it is beneficial to ICF physical experiments if adverse effects are avoided.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
In order to achieve these objects and other advantages, according to the present invention, there is provided a processing method for improving local wettability of a surface of a GDP microsphere, in a manufacturing process of assembling the GDP microsphere and a quartz gas-filled tube, a mask assembly is used to shield the surface of the GDP microsphere, so that a local bonding region on the GDP microsphere, which is matched with the gas-filled tube, is exposed, and then an argon plasma is used to process the exposed local bonding region, thereby improving wettability of an adhesive liquid in the local bonding region, and further improving local bonding performance.
A processing method for avoiding accelerated oxidation of GDP hollow microspheres is characterized in that in the sealing and bonding process of assembling GDP hollow microspheres and a quartz gas-filled tube, a mask component is adopted to shield the surfaces of the GDP hollow microspheres, so that shielded areas of the microspheres cannot be processed when plasma processing is carried out, and when an ultraviolet light curing low-temperature-resistant adhesive is used in the later period, only local bonding areas matched with the gas-filled tube on the GDP hollow microspheres can be exposed in ultraviolet light, and accelerated oxidation of other areas is avoided.
Preferably, the process of masking the surface of the GDP hollow microsphere with the mask assembly is configured to include:
s1, arranging GDP hollow microspheres with gas filling holes on a sample table;
s2, adjusting the position of the mask assembly through the first adjusting assembly so that the through holes in the mask assembly and the inflating holes correspond to each other in space;
and S3, adjusting the height of the sample stage through a second adjusting assembly so that the surface of the GDP hollow microsphere is in contact with the mask assembly.
Preferably, in S1, a conical sinking structure is arranged on the sample stage, and a supporting surface for supporting the GDP hollow microspheres is arranged at the bottom of the sinking structure;
wherein the diameter of the GDP hollow microspheres is configured to be greater than the depth of a conical sunken structure;
an electrostatic adsorption film for limiting the GDP hollow microspheres is arranged on the supporting surface;
the conical surface of the sinking structure is controlled to be 10-60 degrees.
Preferably, in S1, the gas filling hole is processed on the GDP hollow microsphere by a laser device, and the detection of the relevant parameter is completed;
wherein the corresponding pore size is preset according to the outer diameter of the GDP hollow microsphere through the inflation hole, and the outer diameter of the GDP hollow microsphere is 500-5000 microns.
Preferably, in S2, the mask assembly is configured to include masks disposed oppositely and a support frame engaged therewith;
the masks are provided with U-shaped openings matched with each other, so that the masks are in a lap joint shape at the positions of the U-shaped openings under the position adjustment of the first adjusting assembly and the matching of the tweezers, concentric holes matched with the air inflation holes are further formed, and the diameters of the concentric holes are configured to be larger than the target value of the diameter of the glue spots.
Preferably, in S2, the mask assembly is adjusted to be concentric with the gas filling hole under a measuring microscope.
Preferably, the mask is configured to use any one of a polymer film with ultraviolet light protection, a polymer composite film with a carbon coating or a metal coating, an aluminum foil, a tin foil, a copper foil, and the thickness of the mask is generally 0.5 μm to 30 μm;
the supporting frame is made of aluminum or stainless steel, and the thickness of the supporting frame is 50-500 μm;
the mask can be secured to the edge of the support frame by cooperating screws or adhesive.
Preferably, in S2, the first adjusting component is configured to include:
the base is provided with a guide rail with a first internal thread;
the first sliding blocks are respectively arranged at two ends of the mask assembly, and each first sliding block is provided with a sinking groove for accommodating the second sliding block;
the mask component comprises a first slider, a second slider, a first internal thread and a second external thread, wherein the first slider is provided with the first external thread;
first guide holes with second internal threads are respectively formed in the second sliding block, and second external threads for adjusting the mask assembly forwards and backwards are arranged in each first guide hole;
the second adjustment assembly is configured to include: the first guide hole is arranged on the sample table, and the second knob is matched with the first guide hole;
the sample platform adjusts the height of the sample platform through the second guide hole and the internal and external threads on the third knob.
Preferably, the process of performing plasma surface treatment on the local area where the gas filling hole is located by using the plasma treatment machine comprises the following steps:
s4, placing at least one mask device with GDP hollow microspheres in plasma surface treatment equipment;
s5, determining related process parameters of plasma surface treatment according to the frequency of the plasma processor and the cavity volume related factors, and performing plasma surface treatment on the local area where the gas filling hole is located by adopting argon;
and S6, after the plasma surface treatment is finished, pumping out residual gas in the equipment cavity through a vacuum pump, introducing inert gas until the internal pressure and the external pressure of the equipment are equal, and opening a cabin door to take out the mask device.
Preferably, for the plasma surface processor with the radio frequency power supply frequency of 13.56MHz and the cavity volume of 36L, the process parameters are configured to configure the argon flow rate to be 200-400 sccm, the purity of the argon to be not less than 99%, the power to be 300-500 w and the processing time to be 30-300 s.
The invention at least comprises the following beneficial effects: when the surface treatment for improving the wettability is carried out on the GDP hollow microspheres, the non-bonding area (namely the area except the glue spots) is shielded by the shielding mode of the mask assembly, so that the shielded area of the microspheres does not participate in the surface treatment, but the plasma is controlled to only treat the local area near the gas filling holes on the surfaces of the microspheres, thereby improving the wettability and the bonding performance of the adhesive liquid on the local surface of the GDP hollow microspheres, avoiding the microspheres from being subjected to large-area accelerated oxidation and having good controllability. Meanwhile, due to the shielding effect of the mask assembly, the protected surface of the microsphere cannot be irradiated by ultraviolet light in the later bonding process, and the large-area accelerated oxidation is avoided again.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a schematic diagram of a mask assembly mated with a sample stage in accordance with an embodiment of the present invention;
fig. 2 is a partially enlarged schematic view of fig. 1.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
It should be noted that in the description of the present invention, the terms indicating orientation or positional relationship are based on the orientation or positional relationship shown in the drawings only for the convenience of description and simplification of the description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise specifically stated or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are used in a broad sense, and for example, "connected" may be a fixed connection, a detachable connection, an integral connection, a mechanical connection, an electrical connection, a direct connection, an indirect connection through an intermediate medium, and a communication between two elements.
A processing method for improving the local wettability of the surface of a GDP hollow microsphere comprises the steps of firstly shielding the surface of the GDP hollow microsphere by a mask assembly before the GDP hollow microsphere is hermetically bonded with a quartz gas-filled tube, so that only a local area (namely, a local area where a gas-filled hole is located) matched with the gas-filled tube on the GDP hollow microsphere is exposed outside. And then, the exposed local area is treated by adopting argon plasma, so that the wettability of the adhesive liquid to the exposed local area is improved, good bonding sealing performance is further obtained, and simultaneously, the part of the surface of the GDP hollow microsphere which is shielded and protected is prevented from being subjected to plasma treatment to accelerate oxidation. Argon plasma rather than oxygen plasma is adopted for treatment, so that the microspheres are prevented from being oxidized in the treatment process; with masking, the protected areas of the microspheres are not more susceptible to oxidation by forming more "dangling bonds". The bonding area is the area near the gas filling hole on the GDP microsphere, the range of the bonding area is determined according to the size of the target glue spot, and the bonding area is generally slightly larger than the target glue spot so as to prevent the mask plate from being stuck when the size and the shape of the glue spot are controlled to be not ideal. The area of the area is actually the area of a mask hole formed after two mask plates are lapped, other areas of the GDP hollow microsphere except the bonding area are protected by a mask device, then the bonding area is processed by argon plasma, oxygen elements are not introduced in the process of removing low surface energy adsorption substances on the local surface of the microsphere and improving the local surface wettability of the GDP hollow microsphere, meanwhile, only the bonding area is processed locally, and most other areas are protected, so that the microsphere oxidation cannot be accelerated, ultraviolet rays, high-energy particles and the like can be generated in the plasma processing, but the mask can not accelerate the oxidation due to the shielding effect of the mask, and the accelerated oxidation can be avoided in the storage after the processing by further passing the microsphere processed by the mask device.
A processing method for avoiding accelerated oxidation of GDP hollow microspheres is characterized in that in the process of sealing and bonding GDP hollow microspheres and a quartz gas-filled tube, a mask component is adopted to shield the surfaces of the GDP hollow microspheres, when an ultraviolet light curing low-temperature-resistant adhesive is used, only a local bonding area matched with the gas-filled tube on the GDP hollow microspheres is ensured to be exposed in ultraviolet light, accelerated oxidation of other areas in curing is avoided, in the scheme, in the subsequent sealing and bonding process, when the ultraviolet light curing low-temperature-resistant adhesive is used, the mask device can also continuously protect the GDP hollow microspheres, and other parts except the bonding area are prevented from being irradiated by ultraviolet light. The method effectively controls the wettability of the adhesive liquid on the surface of the GDP hollow microsphere, obtains good bonding performance and batch stability, and can not accelerate the oxidation of the microsphere. Therefore, the mask device is added in the existing microsphere processing method, the problem of low-temperature sealing property between the GDP hollow microsphere and the quartz gas-filled tube and the problem of accelerating the oxidation of the microsphere can be effectively solved, and the method is also suitable for the plasma processing of the local surfaces of other types of hydrocarbon polymer microspheres and has wider application range.
In another example, the process of masking the surface of the GDP hollow microsphere with a mask assembly as shown in fig. 1-2 is configured to include:
a. the method comprises the following steps of placing GDP hollow microspheres 10 in a conical sinking surface 12 of a sample table 11, wherein the microspheres automatically reside in the center of the sample table under the action of gravity, in the structure, the height of the conical sinking surface needs to ensure that the small spheres can be exposed, a 500-micrometer platform is arranged below the conical sinking surface of the sample table, and an electrostatic adsorption film is arranged on the platform to realize the fixation of the microspheres and ensure that the alignment position of an inflation hole and a mask is unchanged when the microspheres move in the later period;
b. processing an inflation hole 13 with a set aperture on the GDP hollow microsphere by a laser processing technology, and completing related parameter detection, wherein the related parameter detection is the prior art and is not described herein;
c. by adjusting the 2 left and right displacement knobs and the 2 front and back displacement knobs, the two left and right slide blocks drive the two mask supporting frames to approach to a butt joint state, and the centers of the two U-shaped grooves are positioned right above the GDP hollow microspheres as much as possible;
d. the method comprises the following steps that 2 left and right displacement knobs and 2 front and rear displacement knobs are continuously adjusted under a measuring microscope (a graduated scale is arranged on the measuring microscope, a small ball can be adjusted firstly as required, and a mask can be adjusted later), so that two left and right sliders and two front and rear sliders drive two mask supporting frames to move, and two half masks are lapped through the assistance of precision tweezers, so that two U-shaped grooves on the masks are combined into a basically circular hole, wherein the U-shaped grooves are adopted for lapping, and the reason is that the mask material is too soft, the precision of semicircular butt joint is high, the butt joint size is too precise, the processing is not facilitated, the butt joint is easy to have a seam, and the shielding effect is better due to the lapping mode;
e. adjusting the height of the sample stage by an upper displacement knob and a lower displacement knob under a microscope to enable the gas filling hole on the GDP hollow microsphere to appear in a visual field, and then repeatedly fine-adjusting 5 displacement knobs to enable a round hole formed after the two masks are lapped to be basically concentric with the gas filling hole of the GDP hollow microsphere and enable the upper surface of the GDP hollow microsphere to abut against the lower surface of the mask;
f. placing the mask device with the GDP hollow microspheres in a plasma surface treatment machine, operating the plasma surface treatment machine, and carrying out plasma treatment on the exposed surfaces of the GDP hollow microspheres by adopting argon as process gas;
g. taking out the mask device and the GDP hollow microspheres, and adopting an ultraviolet light curing low temperature resistant adhesive to complete the sealing and bonding of the GDP hollow microspheres and the quartz gas-filled tube to obtain a GDP hollow microsphere/quartz gas-filled tube assembly;
h. and adjusting 2 left and right displacement knobs to enable the left and right slide blocks to drive the two half masks to retreat until the GDP hollow microspheres are completely exposed, and then taking out the GDP hollow microsphere/quartz gas-filled tube assembly to enter a subsequent process.
The structure of the mask device (also referred to as a mask assembly) in the step a is configured to include a mask 14 and a supporting frame 15 matched with the mask 14;
the masks are provided with U-shaped openings 16 matched with each other, so that the masks are in a lap joint shape at the positions of the U-shaped openings under the position adjustment of the first adjusting assembly and the matching of the tweezers, concentric holes matched with the air charging holes are further formed, and the diameters of the concentric holes are configured to be larger than the target value of the diameter of the glue spots.
The mask is configured to be any one of a polymer film with ultraviolet light protection, a polymer composite film with a carbon coating or a metal coating, an aluminum foil, a tin foil and a copper foil, and the thickness of the mask is generally 0.5-30 μm;
the support frame is configured to be made of aluminum or stainless steel, and the thickness of the support frame is configured to be 50 μm-500 μm.
The mask can be fixed to the edge of the support frame by means of cooperating screws or by means of an adhesive.
The outer diameter of the GDP hollow microsphere in the step a is 500-5000 microns.
The laser processing technique in step b is referred to as a laser drilling technique, which is an existing precision processing technique and therefore will not be described in detail.
A mechanism for performing left-right height adjustment on the sample stage is called a first adjusting assembly, and comprises the displacement knob (also called a first knob), the left-right slide block (also called a first slide block), the mask support frame and the U-shaped groove (also called a U-shaped opening) in the step c, and the first adjusting assembly is configured to comprise:
the guide rail fixing device comprises a base 1, a fixing device and a fixing device, wherein a guide rail 2 with first internal threads is arranged on the base 1, and the guide rail is arranged on the base through a mounting screw 3;
each first sliding block is provided with a first knob 5, and the first knob is provided with a first external thread meshed with the first internal thread so as to adjust the position of the mask assembly left and right;
the front end of the left and right displacement knob in the steps c and d is provided with an external thread which is meshed with the thread on the guide rail; meanwhile, the left and right displacement knobs are fixedly connected with the left and right sliding blocks. When the knob is rotated, the guide rail is fixed and does not displace, and the left and right displacement knobs drive the left and right slide blocks and the mask arranged on the slide blocks to displace left and right.
A mechanism for performing front, back, left and right height adjustment on the sample table is called a first adjusting component, a front and back displacement knob 6 (also called a second knob) in steps c and d is positioned in a front and back guide hole (also called a first guide hole) 7, and the front end of the knob is provided with an external thread and is meshed with the internal thread of the front and back guide hole; the guide hole and the internal thread thereof are fixed in position and do not displace, and the front and rear displacement knob drives the front and rear sliders 8 (also called as second sliders) fixed thereon and the mask mounted on the sliders to displace front and rear.
The mask supporting frame in the step c is a frame made of metal such as duralumin or stainless steel, and the thickness of the metal frame is 50-500 mu m (the thickness is too thin and easy to deform); the mask may be a polymer film for ultraviolet light protection, a polymer composite film with a carbon coating or a metal coating, or a metal film such as an aluminum foil, a tin foil, or a copper foil having good ductility, and the thickness of the film or the metal foil is generally 0.5 to 30 μm. Spreading a film or a metal foil on a mask supporting frame, cutting off redundant parts according to the outline dimension structure shown in the specification and the attached drawings, then installing the supporting frame with the mask on a base of a mask device, and fixing the supporting frame with a bar-shaped positioning magnet and a pressing block. When the film or foil used is not spread flat on the support frame, it can also be adhesively secured with a low-viscosity adhesive to prevent warping or wrinkling. The mask may be reused multiple times. Next, under a microscope, two mask supporting frames are made to approach through adjusting 2 left and right displacement knobs and 2 front and back displacement knobs until the mask supporting frames are in a butt joint state, and then two U-shaped grooves are made by adopting a laser processing technology.
And d, forming circular holes after the masks are lapped in the U-shaped grooves in the step c and the step d, wherein the diameter of each circular hole is slightly larger than the target value of the diameter of the glue spot.
The lapping dimension of the mask in the step d is not strictly required, and is generally 30-100 μm according to the rigidity characteristic of the selected mask material.
The sample stage in the step e is a liftable sample stage, is positioned in an upper guide hole and a lower guide hole (also called as a second guide hole), and is adjusted in height through 1 upper displacement knob and lower displacement knob 9 (also called as a third knob). The lower end is provided with an external thread which is meshed with the external thread arranged at the front end of the upper and lower displacement knobs. When the knob is rotated, the position of the knob is fixed and does not generate displacement, and the sample platform can generate vertical displacement in the guide hole.
And e, enabling the upper surface of the sample table in the step e to be a conical sinking surface, and enabling the microspheres to automatically center under the action of gravity after being placed on the sample table. The taper of the conical sinking surface is not strictly required, and is generally 10-60 degrees in consideration of the requirements of microsphere positioning and observation under a microscope.
The plasma surface treatment in the step f comprises the following steps:
f1. opening the vacuum plasma surface treatment equipment to enable the equipment to be in a standby state;
f2. placing a mask device with a GDP hollow microsphere inside in plasma surface treatment equipment; multiple mask devices may be placed simultaneously to process multiple microspheres simultaneously;
f3. determining the technological parameters of plasma surface treatment according to the frequency of the equipment, the volume of the cavity and the like; for a plasma surface processor with the frequency of a radio frequency power supply of 13.56MHz and the volume of a cavity of 36L, the flow rate of argon is 200-400 sccm, the power is 300-500 w, and the processing time is 30-300 s;
f4. after the argon plasma treatment is finished, pumping out residual gas in the equipment cavity through a vacuum pump, and introducing inert gas such as nitrogen or argon until the internal and external pressure intensities of the equipment are equal and the cabin door can be opened;
f5. taking out the mask device to complete the local surface plasma treatment of the GDP hollow microspheres;
and f, the purity of the argon in the step f is not lower than 99%.
The argon flow rate, processing time, power, etc. in step f are related to the model and specification of the vacuum plasma surface treatment apparatus, for example, when the chamber of the apparatus is small, the power and processing time can be as low as 7w and 10s, which are greatly different from the parameters listed in the present invention.
And g, curing the low-temperature resistant adhesive in the step g through ultraviolet irradiation. During the irradiation process, the GDP hollow microspheres are protected by a mask, and only the microsphere surface in the mask hole area is exposed under the irradiation of ultraviolet light.
The invention aims to provide a surface treatment method for improving the surface wettability of GDP hollow microspheres, and oxidation cannot be accelerated. Therefore, a plasma local surface treatment method and a mask device are designed, the device can protect other areas of the GDP hollow microspheres except for the bonding area, then the bonding area is locally treated by adopting argon plasma, and oxygen is not introduced in the process of removing the low surface energy adsorption substances on the surfaces of the microspheres. In the subsequent sealing and bonding process, when the ultraviolet light curing low-temperature-resistant adhesive is adopted, the mask device can also protect the GDP hollow microspheres, so that other parts except the bonding area are prevented from being irradiated by additional ultraviolet light. The method effectively improves the wettability of the adhesive liquid on the surface of the GDP hollow microsphere, obtains good adhesive property and batch stability, and does not accelerate oxidation.
The invention provides an effective surface treatment method of a bonded material from the perspective of improving the surface wettability of GDP hollow microspheres, so that the improvement of gas tightness is facilitated, and the following description and verification are carried out through embodiments:
example 1
The embodiment comprises the following steps:
1. selecting a stainless steel mask supporting frame with the thickness of 50 mu m; polyimide (PI) composite film with aluminum coating is selected as a mask, the thickness of the PI film is 0.5 mu m, and the thickness of the aluminum coating is 30nm. The PI composite film is spread on a mask supporting frame, redundant parts are cut off according to the outline structure shown in the attached drawing of the specification, and then the supporting frame with the mask is installed on a base of a mask device and is fixed by a bar-shaped positioning magnet and a pressing block. Next, under a microscope, the two mask supporting frames are made to approach to each other by adjusting the 2 left and right displacement knobs and the 2 front and rear displacement knobs until the two mask supporting frames are in a butt joint state, and then two U-shaped grooves are formed by adopting a laser processing technology. The diameter of the glue spot of the GDP hollow microsphere/quartz gas-filled tube assembly in this example is targeted to be not more than 50 μm, so the diameter of the U-shaped groove is processed to be 80 μm, and the linear side length of the U-shaped groove is processed to be 30 μm. The assembled mask can be reused for many times, and the mask with the specification is adopted in the embodiment of the invention.
2. Placing GDP hollow microspheres with the outer diameter of 850 micrometers on a sample table, automatically placing the microspheres in the center of the sample table under the action of gravity, then obtaining inflation holes with the diameter of 20 micrometers on the GDP hollow microspheres by a laser processing technology, and completing related parameter detection;
3. by adjusting the 2 left and right displacement knobs and the 2 front and back displacement knobs, the two left and right slide blocks drive the two mask supporting frames to approach to a butt joint state, and the centers of the two U-shaped grooves are positioned right above the GDP hollow microspheres as much as possible;
4. continuously adjusting 2 left and right displacement knobs and 2 front and back displacement knobs under a microscope to enable the two left and right slide blocks and the two front and back slide blocks to drive the two mask supporting frames to move, and overlapping the two half masks by the aid of precision tweezers to enable the two U-shaped grooves on the masks to be combined into a basically circular hole (the overlapping length is about 30 micrometers, and the diameter of the circular hole is about 80 micrometers);
5. adjusting the height of the sample stage under a microscope through an upper displacement knob and a lower displacement knob to enable the gas filling hole on the GDP hollow microsphere to appear in a visual field, and then repeatedly fine-adjusting 5 displacement knobs to enable a round hole formed after the two masks are lapped to be basically concentric with the gas filling hole of the GDP hollow microsphere and enable the upper surface of the GDP hollow microsphere to abut against the lower surface of the mask;
6. placing the mask device with the GDP hollow microspheres in a vacuum plasma surface treatment machine, operating the plasma surface treatment machine, and carrying out plasma treatment on the exposed surfaces of the GDP hollow microspheres by adopting argon as process gas; the radio frequency power supply frequency of the vacuum plasma surface treatment machine is 13.56MHz, the cavity volume is 36L, the argon flow rate is 200sccm, the power is 300w, and the treatment time is 300s;
7. taking out the mask device and the GDP hollow microspheres, and adopting an ultraviolet light curing low temperature resistant adhesive to complete the sealing and bonding of the GDP hollow microspheres and the quartz gas-filled tube to obtain a GDP hollow microsphere/quartz gas-filled tube assembly;
8. and adjusting 2 left and right displacement knobs to enable the left and right slide blocks to drive the two half masks to retreat until the GDP hollow microspheres are completely exposed, and then taking out the GDP hollow microsphere/quartz gas-filled tube assembly to enter a subsequent process.
The low-temperature sealing performance test result shows that the leakage rate of the component at 18K is 2.1 multiplied by 10 < -6 > Pa.L/s, and the ICF experimental requirement is met.
Example 2
Example 2 the procedure of example 1 was substantially the same, with the main difference that the GDP hollow microspheres had an outer diameter of 800 microns; the plasma treatment process parameters are as follows: the argon flow rate was 250sccm, the power was 350w, and the process time was 240s.
The low-temperature sealing performance test result shows that the leakage rate of the component at 18K is 2.4 multiplied by 10 < -6 > Pa.L/s, and the ICF experimental requirement is met.
Example 3
Example 3 the procedure of example 1 is essentially the same, with the main difference that the outer diameter of the GDP hollow microspheres is 2000 μm; the plasma treatment process parameters are as follows: the argon flow rate was 400sccm, the power was 500w, and the treatment time was 30s.
The low-temperature sealing performance test result shows that the leakage rate of the component at 18K is 3.1 multiplied by 10 < -6 > Pa.L/s, and the ICF experimental requirement is met.
The invention provides a method for improving the local wettability and the adhesion of the surface of a GDP hollow microsphere. Before the GDP hollow microspheres are sealed and bonded with the quartz gas-filled tube, firstly, the surface of the GDP hollow microspheres is shielded by a mask component, so that only a local area (namely, a local area where a gas-filled hole is located) matched with the gas-filled tube on the GDP hollow microspheres is exposed outside. And then, the exposed local area is treated by adopting argon plasma, so that the wettability of the adhesive liquid to the exposed local area is improved, good sealing performance is further obtained, and meanwhile, the part of the surface of the GDP hollow microsphere which is shielded and protected is prevented from being subjected to plasma treatment to accelerate oxidation. In the subsequent sealing and bonding process, when the ultraviolet curing low-temperature-resistant adhesive is adopted, the mask device protects the GDP hollow microspheres again, so that the shielded and protected part of the GDP hollow microspheres is prevented from being irradiated by ultraviolet light to accelerate oxidation.
The invention provides a method for improving the surface local wettability and the adhesiveness of GDP hollow microspheres and simultaneously avoiding the microspheres from being oxidized in a large area in an accelerated manner, namely, a non-adhesive area (namely, an area except glue spots) is shielded by a mask assembly so as to control the area of plasma treatment and the area of ultraviolet irradiation. Therefore, only the exposed local area on the surface of the GDP hollow microsphere is treated by the plasma, so that the wettability and the bonding property are improved, the shielded area on the surface of the microsphere cannot be treated by the plasma, and the blocked area cannot be irradiated by ultraviolet light in the bonding process in the later period, so that the wettability and the bonding property of the adhesive liquid on the surface of the GDP hollow microsphere are finally improved, and the GDP hollow microsphere is prevented from being oxidized in an accelerated manner. The wettability and the bonding effect of the local surface of the GDP hollow microsphere are controlled by the plasma treatment process parameters.
The above scheme is merely illustrative of a preferred example, and is not limiting. In the implementation of the invention, appropriate replacement and/or modification can be carried out according to the requirements of users.
The number of apparatuses and the scale of the process described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be apparent to those skilled in the art.
While embodiments of the invention have been disclosed above, it is not intended to be limited to the uses set forth in the specification and examples. It can be applied to all kinds of fields suitable for the present invention. Additional modifications will readily occur to those skilled in the art. Therefore, the invention is not to be limited to the specific details and illustrations shown and described herein, without departing from the general concept as defined by the claims and their equivalents.
Claims (9)
1. A processing method for improving local wettability of the surface of a GDP hollow microsphere is characterized in that in the preparation process of assembling the GDP hollow microsphere and a quartz gas-filled tube, a mask assembly is adopted to shield the surface of the GDP hollow microsphere, so that a local bonding area matched with the gas-filled tube on the GDP hollow microsphere is exposed outside, and then argon plasma is adopted to process the exposed local bonding area, so that wettability of adhesive liquid in the local bonding area is improved, and further local bonding performance is improved;
the process of shielding the surface of the GDP hollow microspheres by using the mask assembly is configured to comprise the following steps:
s1, arranging GDP hollow microspheres with gas filling holes on a sample table;
s2, adjusting the position of the mask assembly through the first adjusting assembly so that the through holes in the mask assembly and the inflating holes correspond to each other in space;
and S3, adjusting the height of the sample stage through a second adjusting assembly so that the surface of the GDP hollow microsphere is in contact with the mask assembly.
2. A processing method for avoiding accelerated oxidation of GDP hollow microspheres is characterized in that in the sealing and bonding process of assembling GDP hollow microspheres and a quartz gas-filled tube, a mask assembly is adopted to shield the surfaces of the GDP hollow microspheres, so that shielded areas of the microspheres cannot be processed when plasma processing is carried out, and when an ultraviolet curing low-temperature-resistant adhesive is used at the later stage, only local bonding areas on the GDP hollow microspheres, which are matched with the gas-filled tube, are exposed in ultraviolet light, and accelerated oxidation of other areas is avoided;
the process of shielding the surface of the GDP hollow microspheres by using the mask assembly is configured to comprise the following steps:
s1, arranging GDP hollow microspheres with air inflation holes on a sample table;
s2, adjusting the position of the mask assembly through the first adjusting assembly so that the through holes in the mask assembly and the inflating holes correspond to each other in space;
and S3, adjusting the height of the sample stage through a second adjusting assembly so that the surface of the GDP hollow microsphere is in contact with the mask assembly.
3. The processing method according to claim 1 or 2, wherein in S1, a conical sunken structure is arranged on the sample stage, and the bottom of the sunken structure is provided with a supporting surface for supporting the GDP hollow microspheres;
wherein the diameter of the GDP hollow microspheres is configured to be greater than the depth of a conical sunken structure;
an electrostatic adsorption film for limiting the GDP hollow microspheres is arranged on the supporting surface;
the conical surface of the sinking structure is controlled to be 10-60 degrees.
4. The process of claim 1 or 2, wherein in S1, the gas filling hole is processed on the GDP hollow microsphere by a laser device, and the relevant parameter detection is completed;
wherein the corresponding pore size is preset according to the outer diameter of the GDP hollow microsphere through the inflation hole, and the outer diameter of the GDP hollow microsphere is 500-5000 microns.
5. The process of claim 1 or 2, wherein in S2, the mask assembly is configured to include the mask in an opposing arrangement and a support frame cooperating therewith;
the masks are provided with U-shaped openings matched with each other, so that the masks are in a lap joint shape at the positions of the U-shaped openings under the position adjustment of the first adjusting assembly and the matching of the tweezers, concentric holes matched with the air charging holes are further formed, and the diameters of the concentric holes are configured to be larger than the target value of the diameter of the glue spot;
in S2, the mask assembly is adjusted to be concentric with the gas filled hole under a measuring microscope.
6. The process of claim 5, wherein the mask is configured to use any one of a polymer film with ultraviolet light protection, a polymer composite film with a carbon coating or a metal coating, an aluminum foil, a tin foil, a copper foil, and the thickness of the mask is generally 0.5 μm to 30 μm;
the supporting frame is made of aluminum or stainless steel, and the thickness of the supporting frame is 50-500 μm;
the mask can be fixed to the edge of the support frame by means of cooperating screws or adhesive.
7. The processing method of claim 1 or 2, wherein in S2 the first adjustment component is configured to comprise:
the base is provided with a guide rail with a first internal thread;
the first sliding blocks are respectively arranged at two ends of the mask component, and each first sliding block is respectively provided with a sunk groove for accommodating the second sliding block;
the mask component comprises a first slider, a second slider, a first internal thread and a second external thread, wherein the first slider is provided with the first external thread;
first guide holes with second internal threads are respectively formed in the second sliding block, and second external threads for adjusting the mask assembly forwards and backwards are arranged in each first guide hole;
the second adjustment assembly is configured to include: the first guide hole is arranged on the sample table, and the second knob is matched with the first guide hole;
the sample table adjusts the height of the sample table through the second guide hole and the internal and external threads on the third knob.
8. The process of claim 1, wherein the plasma surface treatment of the local region where the gas filling hole is located by the plasma treatment machine comprises:
s4, placing at least one mask device with GDP hollow microspheres in plasma surface treatment equipment;
s5, determining related process parameters of plasma surface treatment according to the frequency of the plasma treatment machine and the cavity volume related factors, and performing plasma surface treatment on the local area where the gas filling hole is located by adopting argon;
and S6, after the plasma surface treatment is finished, pumping out residual gas in the equipment cavity through a vacuum pump, introducing inert gas until the internal pressure and the external pressure of the equipment are equal, and opening a cabin door to take out the mask device.
9. The processing method according to claim 8, wherein in S5, for the plasma surface processing machine having a frequency of the rf power supply of 13.56MHz and a chamber volume of 36L, the process parameters are configured to set an argon flow rate of 200 to 400 seem, a purity of argon of not less than 99%, a power of 300w to 500w, and a processing time of 30S to 300S.
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|---|---|---|---|---|
| US5254372A (en) * | 1991-02-27 | 1993-10-19 | Nichols Technologies, Inc. | Method and apparatus for plasma treatment of a filament |
| JP2005142227A (en) * | 2003-11-04 | 2005-06-02 | Matsushita Electric Ind Co Ltd | Plasma processing method and processing apparatus |
| WO2017135571A1 (en) * | 2016-02-02 | 2017-08-10 | Plasmapp Co., Ltd. | Linear plasma generator for selective surface treatment |
| WO2018008806A1 (en) * | 2016-07-06 | 2018-01-11 | 주식회사 플라즈맵 | Separation film processing method for secondary battery using atmospheric pressure dielectric barrier discharge plasma |
| CN112516930A (en) * | 2020-11-16 | 2021-03-19 | 中国工程物理研究院激光聚变研究中心 | Method for preparing hollow microspheres with high sphericity, high surface finish and high degradation performance |
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2021
- 2021-11-26 CN CN202111419033.6A patent/CN114106391B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5254372A (en) * | 1991-02-27 | 1993-10-19 | Nichols Technologies, Inc. | Method and apparatus for plasma treatment of a filament |
| JP2005142227A (en) * | 2003-11-04 | 2005-06-02 | Matsushita Electric Ind Co Ltd | Plasma processing method and processing apparatus |
| WO2017135571A1 (en) * | 2016-02-02 | 2017-08-10 | Plasmapp Co., Ltd. | Linear plasma generator for selective surface treatment |
| WO2018008806A1 (en) * | 2016-07-06 | 2018-01-11 | 주식회사 플라즈맵 | Separation film processing method for secondary battery using atmospheric pressure dielectric barrier discharge plasma |
| CN112516930A (en) * | 2020-11-16 | 2021-03-19 | 中国工程物理研究院激光聚变研究中心 | Method for preparing hollow microspheres with high sphericity, high surface finish and high degradation performance |
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