CN210571846U - Nanoparticle size measurement system - Google Patents

Abstract

The application provides a nanoparticle size measurement system. A first light blocking structure and a second light blocking structure are placed in the matching fluid. The first light blocking structure is arranged on the positive extension line of the incident light beam and used for absorbing and reflecting the light beam, so that the light beam cannot reach the junction of the wall surface of the matching pool and air and is reflected. The second light blocking structure is arranged on a reverse extension line of scattered light beams received by the scattering light through holes and used for absorbing and reflecting the scattered light beams on complementary angles of the measuring receiving angles, so that the scattered light beams cannot reach the junction of the wall surface of the matching pool and air and are reflected. The influence of reflected light on the wall surface of the sample cell in the traditional nanoparticle particle size measuring system can be greatly reduced through the matching fluid, the first light blocking structure and the second light blocking structure, reflected light information is prevented from being mixed into scattered light signals of which the angles are received by the multiple scattered light through holes, and therefore the accuracy of a measuring result is greatly improved.

Description

Nanoparticle size measurement system

Technical Field

The application relates to the technical field of measurement, in particular to a nanoparticle size measurement system.

Background

The particle size measurement of the nano particles mainly comprises an electron microscope and various dynamic light scattering nano particle size measurement methods developed based on a dynamic light scattering theory, when the nano particles are suspended in liquid, random motion can be generated by disordered impact of a large number of surrounding liquid molecules, and the motion of the particles is called brownian motion. When the nano particles do brownian motion in the liquid, the scattered light of the nano particles pulsates. Since the magnitude of the pulsation frequency is related to the diffusion coefficient of the nanoparticles, and the diffusion coefficient is related to the size of the nanoparticles, the particle size of the nanoparticles can be measured using a dynamic light scattering method.

However, in the conventional nanoparticle particle size measurement system, the light beam of the incident light beam passing through the scattering center is reflected in the process from the optically dense medium to the optically thinner medium, i.e., reflected at the interface between the wall surface of the sample cell and the air. The reflected light beam can be received by the scattered light receiving device in the reflection direction, so that reflected light information is mixed into the scattered light signal of the self angle received by the scattered light receiving device, measurement errors are caused, and the measurement result of the traditional nanoparticle particle size measurement system is inaccurate.

SUMMERY OF THE UTILITY MODEL

Based on this, it is necessary to provide a nanoparticle size measurement system to solve the problem of inaccurate measurement result of the conventional nanoparticle size measurement system.

The application provides a nanoparticle particle size measurement system includes scattering generating device, matching pond, sample cell, matching liquid, end cover, first light blocking structure supporting part, first light blocking structure and second light blocking structure. The scattering generating device is used for enabling the to-be-detected nano particles to scatter at various angles under the interaction. The scatter generating device includes a first annular side plate. The first annular side plate surrounds to form a first containing space with a first opening. The first annular side plate is provided with an incident light through hole and a plurality of scattered light through holes. The incident light through hole and the scattering light through holes are arranged on the same horizontal plane. And the axes of the incident light through holes and the axes of the scattering light through holes intersect at the same scattering center point.

The matching pool is arranged in the first accommodating space. The matching tank includes a second receiving space formed with a second opening. The sample cell is arranged in the second accommodating space and used for accommodating a sample solution. And the incident light beam irradiates the sample cell through the incident light through hole to form a scattered light beam. The plurality of scattering light through holes are used for enabling the scattering light beams to pass through. The matching fluid is arranged in the second accommodating space and surrounds the sample cell. And the refractive index of the matching fluid is the same as that of the wall surface of the sample cell. The end cover is matched with the first opening. And the end cover is provided with a first placing hole. The diameter of the sample cell is smaller than that of the first placement hole. The first light blocking structure supporting part is arranged between the sample cell and the matching cell. The first light blocking structure supporting part is connected with the end cover. The first light blocking structure is used for absorbing and reflecting the light beam after passing through the sample cell. The first light blocking structure is arranged between the sample cell and the matching cell. The first light blocking structure is connected with the first light blocking structure supporting part. And the first light blocking structure is arranged on the incident light beam forward extension line. The second light blocking structure is arranged between the sample cell and the matching cell. The second light blocking structure is connected with the end cover. And the second light blocking structure is arranged on the reverse extension line of the scattered light beams received by the scattered light through holes.

In one embodiment, the second light blocking structure is provided with a through hole. The axes of the through hole, the incident light through hole and the scattering light through holes are intersected at the same scattering center point. The included angle between the axis of the through hole and the axis of the incident light through hole at the scattering center point is 90 degrees.

In one embodiment, the nanoparticle size measurement system further comprises an incident light device. The incident light device is used for adjusting incident light beams to enter the scattering generation device through the incident light through hole. The incident light device includes a first Glan-Thomson prism and a first prism tuning structure. The first Glan Thomson prism is arranged on the first prism adjusting structure, and the position of the first Glan Thomson prism is adjusted by the first prism adjusting structure, so that an incident light beam is incident to the incident light through hole through the first Glan Thomson prism.

In one embodiment, the nanoparticle size measurement system further comprises a plurality of scattered light receiving devices. Each scattered light receiving device corresponds to one scattered light through hole and is used for receiving scattered light beams emitted by the scattered light through holes. And the receiving light paths of the scattered light receiving devices intersect at the same scattering center point of the sample cell.

In one embodiment, each of the scattered light receiving devices includes a mirror, a fiber focus lens, and an optical fiber. One of the mirrors corresponds to one of the scattering light through holes. The reflecting mirror is arranged on a scattered light beam light path emitted by the scattered light through hole and is used for reflecting the scattered light beam at an incidence angle of 45 degrees. The optical fiber focusing lens is arranged on a scattered light beam light path reflected by the reflecting mirror and used for focusing the scattered light beam. The optical fiber is connected with the optical fiber focusing lens and used for transmitting the scattered light beam received by the optical fiber focusing lens to the photon counter through the optical fiber.

In one embodiment, each of the scattered light receiving devices further comprises a second glanston prism and a second prism adjustment structure. The second Glan Thomson prism is disposed on the second prism adjustment structure. Adjusting a position of the second granthomson prism by the second prism adjustment structure so that the scattered light beam is incident to the mirror through the second granthomson prism.

In one embodiment, the nanoparticle size measurement system further comprises a charge coupled device camera. The CCD camera is arranged opposite to the first placing hole and used for recording image information of the incident light beams and the scattered light beams converged at the scattering center point of the sample cell in real time.

In one embodiment, the nanoparticle size measurement system further includes a plurality of third placement holes. The plurality of third placing holes are formed in the end cover and used for placing a temperature sensor so as to monitor the temperature in the second containing space in real time.

In one embodiment, the nanoparticle size measurement system further comprises a temperature control module and a plurality of temperature control structures. The temperature control module is connected with the temperature sensor and used for acquiring the temperature in the second accommodating space. The plurality of temperature control structures are arranged on the outer wall, far away from the first containing space, of the first annular side plate, and the plurality of temperature control structures are connected with the temperature control module. The temperature control module regulates and controls the plurality of temperature control structures according to the temperature change in the second accommodating space, so that the temperature in the second accommodating space is stable.

In one embodiment, the end cap is provided with a plurality of second placing holes for placing matching liquid pipelines to convey the matching liquid.

The application provides a above-mentioned nanoparticle particle size measurement system. The sample cell, the matching fluid, the first light blocking structure and the second light blocking structure are all arranged in the second containing space formed by surrounding the matching cell. At this time, the incident light beam is incident to the sample cell through the incident light through hole via the matching fluid. And the incident beam enters the matching fluid through the cell wall of the sample cell after passing through the scattering center. The scattered light beam passing through the scattering center propagates in the matching fluid medium.

The refractive index of the matching fluid is close to that of the wall surface of the sample cell. The matching fluid can be decalin with a refractive index close to that of the glass wall surface, and scattered light beams passing through the wall surface of the sample cell can still be considered to be transmitted in a medium with a refractive index close to that of the glass wall surface. At this time, the influence of the wall surface of the sample cell is eliminated by the matching fluid.

The first light blocking structure and the second light blocking structure are placed in the matching fluid. The first light blocking structure is arranged on a positive extension line of an incident light beam, namely, the first light blocking structure is used for absorbing and reflecting the light beam (the incident light beam after passing through a scattering center) transmitted in the matching fluid medium, so that the light beam cannot reach the junction of the wall surface of the matching pool and air and is reflected. At this time, the first light blocking structure is light blocking (having passed through the scattering center) after 0 ° incidence. The second light blocking structure is arranged on a reverse extension line of the scattered light beams received by the scattered light through holes. The reverse extension lines of the scattered light beams received by the scattered light through holes are complementary angle directions of the measured receiving angles. The second light blocking structure is used for absorbing and reflecting the scattered light beams at the complementary angle of the measuring receiving angle which are transmitted in the matching fluid medium, so that the scattered light beams at the complementary angle cannot reach the boundary between the wall surface of the matching pool and the air to be reflected.

Therefore, the influence of the reflected light on the wall surface of the sample cell in the traditional nanoparticle particle size measurement system can be greatly reduced through the matching fluid, the first light blocking structure and the second light blocking structure. Meanwhile, reflected light information can be prevented from being mixed into scattered light signals of which the angles are received by the plurality of scattered light through holes through the matching fluid, the first light blocking structure and the second light blocking structure, so that the accuracy of the measurement result of the nanoparticle particle size measurement system is improved.

Drawings

FIG. 1 is a schematic diagram of the overall structure of a nanoparticle size measurement system provided herein;

fig. 2 is a schematic cross-sectional structure diagram of a scattering generation device provided in the present application;

fig. 3 is a schematic cross-sectional structure diagram of a second scattering generation device provided in the present application;

fig. 4 is a schematic cross-sectional structure diagram of a scattering generation device provided in the present application;

fig. 5 is a schematic cross-sectional structure diagram of a scattering generation device provided in the present application;

fig. 6 is a schematic diagram of an optical path in the scattering generation apparatus provided in the present application;

fig. 7 is a schematic cross-sectional structure diagram five of the scattering generation device provided in the present application;

FIG. 8 is a first schematic view of the overall structure of the scattering generation device provided in the present application;

fig. 9 is a schematic view of the overall structure of the scattering generation device provided in the present application;

fig. 10 is a schematic diagram illustrating an overall structure of an incident light device provided in the present application;

fig. 11 is a schematic view of the overall structure of a scattered light receiving device provided in the present application;

fig. 12 is a schematic structural diagram of a ccd camera provided herein;

fig. 13 is a schematic overall structure diagram of a nanoparticle size measuring instrument provided in the present application.

Description of the reference numerals

Nanoparticle particle size measurement system 100, scattering generation device 10, matching cell 150, sample cell 180, matching fluid 153, end cap 140, first light blocking structure support 161, first light blocking structure 160, second light blocking structure 170, first annular side plate 130, first opening 131, first receiving space 132, incident light through hole 110, scattered light through hole 120, second opening 151, second receiving space 152, through hole 171, incident light device 20, first glan tomson prism 210, first prism adjusting structure 220, scattered light receiving device 30, reflector 310, fiber focusing lens 320, optical fiber 330, isolation plate hole 340, second glan tomson prism 350, second prism adjusting structure 360, charge coupled device camera 40, camera support frame 410, temperature control structure 190, temperature control module 191, laser 50, attenuator 60, second placing hole 142, sample stage 181, sample, The device comprises a support rod 162, an incident diaphragm hole 111, a first reflector 710, a second reflector 720, a lens 730, a heat exchanger 80, a support seat 810, a photomultiplier 820, a correlator 830, a nanoparticle size measuring instrument 200, an instrument housing 90 and an instrument accommodating space 910.

Detailed Description

In order to make the objects, technical solutions and advantages of the present application more apparent, the present application is further described in detail below by way of embodiments and with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.

The numbering of the components as such, e.g., "first", "second", etc., is used herein only to distinguish the objects as described, and does not have any sequential or technical meaning. The term "connected" and "coupled" when used in this application, unless otherwise indicated, includes both direct and indirect connections (couplings). In the description of the present application, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present application and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be considered as limiting the present application.

In this application, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through intervening media. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.

Referring to fig. 1-9, a nanoparticle size measurement system 100 includes a scatter generating device 10. The scattering generating device 10 includes a matching cell 150, a sample cell 180, a matching fluid 153, an end cap 140, a first light blocking structure support 161, a first light blocking structure 160, and a second light blocking structure 170. Within the sample cell 180 of the scattering generation device 10, the nanoparticles in the sample solution undergo scattering at various angles under interaction. The scatter generating device 10 comprises a first annular side plate 130. The first annular side plate 130 encloses a first receiving space 132 having a first opening 131. The first annular side plate 130 is provided with an incident light through hole 110 and a plurality of scattered light through holes 120. The incident light passing hole 110 and the scattering light passing holes 120 are disposed at the same level. And the axis of the incident light through hole 110 intersects with the axes of the scattering light through holes 120 at the same scattering center point.

The matching tank 150 is disposed in the first receiving space 132. The matching reservoir 150 includes a second receiving space 152 formed with a second opening 151. The sample cell 180 is disposed in the second receiving space 152 for placing a sample solution. The incident light beam irradiates the sample cell 180 through the incident light through hole 110 to form a scattered light beam. The plurality of scattered light pass through holes 120 are used to pass scattered light beams. The matching fluid 153 is disposed in the second receiving space 152 and surrounds the sample cell 180. And the refractive index of the matching fluid 153 is the same as that of the wall surface of the sample cell 180. The end cap 140 is disposed to match the first opening 131. And the end cap 140 is provided with a first placing hole 141. The diameter of the sample cell 180 is smaller than that of the first placing hole 141. The first light blocking structure supporting part 161 is disposed between the sample cell 180 and the matching cell 150. The first light blocking structure supporting part 161 is connected to the end cap 140. The first light blocking structure 160 is used for absorbing and reflecting the light beam after passing through the sample cell 180. The first light blocking structure 160 is disposed between the sample cell 180 and the matching cell 150. The first light blocking structure 160 is connected to the first light blocking structure supporting portion 161. And the first light blocking structure 160 is disposed on the forward extension line of the incident light beam. The second light blocking structure 170 is disposed between the sample cell 180 and the matching cell 150. The second light blocking structure 170 is connected to the end cap 140. And the second light blocking structure 170 is disposed on a reverse extension line of the scattered light beam received by the scattered light through holes 120.

The sample cell 180, the matching fluid 153, the first light blocking structure 160 and the second light blocking structure 170 are all disposed in the second receiving space 152 surrounded by the matching cell 150. At this time, the incident light beam is incident to the sample cell 180 through the incident light through hole 110 via the matching fluid 153. The incident beam passes through the scattering center and then enters the matching fluid 153 through the cell wall of the sample cell 180. The light beam passing through the scattering center propagates in the matching fluid medium.

The refractive index of the matching fluid 153 is close to that of the wall surface of the sample cell 180. The matching fluid 153 may be decalin with a refractive index similar to that of the glass wall surface, and it is considered that the light beam passing through the wall surface of the sample cell 180 still propagates in a medium with a refractive index similar to that of the glass wall surface. At this time, the influence of the wall surface of the sample cell 180 is eliminated by the matching fluid 153.

The first light blocking structure 160 and the second light blocking structure 170 are disposed in the matching fluid 153. The first light blocking structure 160 is disposed on a forward extension line of an incident light beam, that is, the first light blocking structure 160 is used to absorb and reflect a light beam (a light beam passing through a scattering center) propagating in the medium of the matching fluid 153, so that the light beam cannot reach a boundary between the wall surface of the matching cell 150 and air and is reflected. At this time, the first light blocking structure 160 is light blocked (already passing through the scattering center) after 0 ° incidence. The second light blocking structure 170 is disposed on a reverse extension line of the scattered light beam received by the scattered light through holes 120. The reverse extension of the scattered light beam received by the plurality of scattered light pass-through holes 120 is the complementary angular direction of the measured acceptance angle. The second light blocking structure 170 is used for absorbing and reflecting the scattered light beam at the complementary angle of the measurement receiving angle propagating in the medium of the matching fluid 153, so that the scattered light beam at the complementary angle cannot reach the boundary between the wall surface of the matching cell 150 and the air and is reflected.

Therefore, the influence of the reflected light from the wall of the sample cell in the conventional nanoparticle size measuring system can be greatly reduced by the matching fluid 153, the first light blocking structure 160 and the second light blocking structure 170. Meanwhile, the matching fluid 153, the first light blocking structure 160 and the second light blocking structure 170 may prevent the scattering light through holes 120 from mixing with the reflected light information in the scattering light signals received from their own angles, thereby improving the accuracy of the measurement result of the nanoparticle size measurement system 100.

In one embodiment, the axis of the incident light through hole 110 and the axes of the plurality of scattered light through holes 120 intersect at the same scattering center point. The incident light through hole 110 and the scattering light through holes 120 are disposed on the same horizontal plane, so as to intersect the incident light and the scattering light at the same center point. The nanoparticle size measurement system 100 can simultaneously measure the same scattering center of the nanoparticles to be measured at a plurality of angles, can obtain the particle scattering rule from the same scattering center, and is more accurate in multi-angle measurement and analysis, so that the nanoparticle size measurement system 100 is short in sampling time, and the measurement precision is improved.

In one embodiment, the first light blocking structure supporting portion 161 is detachably connected to the end cap 140. The first photoresist structure supporting portion 161 is used for fixedly supporting the first photoresist structure 160. The second light blocking structure 170 is detachably connected to the end cap 140. The nanoparticle size measurement system 100 further includes a sample stage 181, and the sample stage 181 is disposed in the second accommodating space 152.

A sample cell groove is formed in one end, close to the sample cell 180, of the sample table 181, and is used for placing the sample cell 180. The sample cell 180 is supported and fixed by the sample stage 181. The nanoparticle size measuring system 100 further includes a support bar 162 disposed corresponding to the first light blocking structure support 161, wherein the support bar 162 is detachably disposed on the end cap 140. The support bar 162 is provided with an entrance diaphragm aperture 111. At this time, the incident light is irradiated to the sample cell 180 through the incident light through hole 110 and the incident light diaphragm hole 111. Meanwhile, the sample stage 181, the sample cell 180 and the matching cell 150 are coaxially arranged, so that scattering signals collected at multiple angles can be ensured to come from the same scattering center.

Referring to fig. 6, in one embodiment, the second light blocking structure 170 is provided with a through hole 171. The axes of the through hole 171, the incident light through hole 110, and the scattered light through holes 120 intersect at the same scattering center point. The angle between the axis of the through hole 171 and the axis of the incident light through hole 110 at the scattering center point is 90 °.

When the measurement receiving angle is 90 °, the included angle between the axis of the scattering light through hole 120 corresponding to 90 ° and the axis of the incident light through hole 110 at the scattering center point is 90 °. At this time, the complementary angle at the measurement acceptance angle of 90 ° is still 90 °, and the scattered light beam at the complementary angle of the measurement acceptance angle has an influence on the measurement result of the nanoparticle diameter measurement system 100. Therefore, the accuracy of the measurement result of the nanoparticle size measuring system 100 is ensured by providing the through hole 171 on the second light blocking structure 170 for receiving the scattered light beam in the direction with the complementary angle of the measurement receiving angle of 90 °.

Referring to fig. 8, in one embodiment, the end cap 140 is provided with a plurality of second placing holes 142 for placing matching liquid pipelines to deliver the matching liquid 153.

The number of the plurality of second placing holes 142 may be 2. One of the second placing holes 142 is used for placing a matching fluid pipeline, and the matching fluid 153 is input into the matching tank 150. The other second placing hole 142 is used for placing a matching liquid pipeline, so that the matching liquid 153 is output from the matching tank 150. At this time, the matching fluid 153 may be circulated through the plurality of second placing holes 142 and the matching fluid pipe, so as to facilitate the renewal of the matching fluid 153 in the matching tank 150.

Referring to fig. 10, in one embodiment, the nanoparticle size measurement system 100 further includes an incident light device 20. The incident light device 20 is used to adjust the incident light beam to enter the scattering generation device 10 through the incident light through hole 110. The incident light device 20 includes a first glan tomson prism 210 and a first prism adjustment structure 220. The first glan tomson prism 210 is disposed on the first prism adjustment structure 220. The position of the first glan tomson prism 210 is adjusted by the first prism adjustment structure 220 so that an incident light beam is incident to the incident light through hole 110 through the first glan tomson prism 210.

The first prism adjusting structure 220 includes a supporting base 221, an adjusting base 222, and an adjusting shaft 223. The adjusting table 222 is disposed on the supporting base 221, and the adjusting shaft 223 is slidably connected to the adjusting table 222. The first glan tomson prism 210 is disposed on the adjusting stage of the first prism adjusting structure 220, and the position of the adjusting stage 222 is controlled by an adjusting shaft 223, so that an incident light beam is incident to the incident light through hole 110 via the first glan tomson prism 210. The first Glan-Thompson prism 210(Glan-Thompson) is disposed on the incident light path to obtain vertically polarized incident light, and at this time, the incident light beam passes through the first Glan-Thompson prism 210 to form vertically polarized incident light and is incident to the incident light through hole 110.

A lens 730 is disposed between the incident light device 20 and the scattering generation device 10. The lens 730 focuses vertically polarized incident light, and the light is incident to the sample cell 180 of the scattering generation device 10 through the incident light through hole 110.

Referring to fig. 1, in one embodiment, the nanoparticle size measurement system 100 further includes a laser 50 and an attenuator 60. The laser 50 is used to emit an incident beam. The attenuator 60 is disposed between the incident light device 20 and the laser 50. The attenuator 60 adjusts the incident beam emitted from the laser 50, and the incident beam adjusted by the attenuator 60 is incident to the incident light via 110 through the incident light device 20.

Wherein the laser 50 is a high power He-Ne laser. The attenuator 60 is an attenuator sheet, and can realize adjustable power.

The nanoparticle size measurement system 100 further includes a first mirror 710 and a first mirror 720. The first mirror 710 may be used to adjust the direction of incident light emitted by the laser 50. The incident light modulated by the first mirror 710 is power-modulated by the attenuator 60. The first mirror 720 may be used to adjust the direction of incident light passing through the attenuator 60. The incident light modulated by the first reflector 720 is incident to the incident light device 20.

In one embodiment, the nanoparticle size measurement system 100 further includes a plurality of scattered light receiving devices 30. The plurality of scattered light receiving means 30 collect scattered light signals emanating from scattering centers. Each scattered light receiving device 30 corresponds to one scattered light through hole 120, and is used for receiving the scattered light beams emitted by the scattered light through holes 120. The receiving light paths of the scattered light receiving devices 30 intersect at the same scattering center point of the sample cell 180. One of the scattered light receiving devices 30 corresponds to one of the scattered light passing holes 120 for receiving scattered light scattered by the solution containing nanoparticles from different angles.

Referring to fig. 11, in one embodiment, each of the scattered light receiving devices 30 includes a mirror 310, a fiber focusing lens 320, and an optical fiber 330. One of the mirrors 310 corresponds to one of the scattering light passing holes 120. The reflecting mirror 310 is disposed on the optical path of the scattered light beam emitted from the scattered light through hole 120, and is configured to reflect the scattered light beam at an incident angle of 45 °. The optical fiber focusing lens 320 is disposed on the scattered light beam light path reflected by the reflecting mirror 310, and is configured to focus the scattered light beam. The optical fiber 330 is connected to the fiber focus lens 320, and is configured to transmit the scattered light beam received by the fiber focus lens 320 to the photon counter through an optical fiber.

The scattered light beam emitted from the scattered light through hole 120 is received by the combination of the fiber focusing lens 320 and the optical fiber 330. The light flux amount and the convenience of use of the scattered light receiving device 30 are increased while satisfying the requirement of spatial coherence. Meanwhile, the optical fiber focusing lens 320 has a focusing function, so that the light intensity of the received signal is greatly improved, and the received signal can be focused to the center of the sample cell 180.

The photomultiplier tube 820 and the optical fiber 330 are connected by an optical fiber. The light intensity information obtained by the photomultiplier 820 is adjusted in real time to reach the maximum light intensity at each receiving angle, so as to ensure the highest coincidence degree of the scattering centers and ensure that the receiving light paths of the scattered light receiving device 30 intersect at the same scattering center point of the sample cell 180.

One of the photomultiplier tubes 820 is connected to one of the scattered light receiving devices 30 for detecting the signal power of the light pulse. The correlator 830 is provided with a plurality of channels, and one channel is connected with one photomultiplier 820 through an optical fiber, so as to obtain light intensity autocorrelation functions of a plurality of scattering angles and realize signal conversion, transmission and correlation operation. And finally, carrying out inverse calculation on the particle size of the nano particles in a computer, and further outputting a particle size measurement result.

The correlator 830 may be a correlation receiver, a tool that uses correlation properties of the signal to extract the desired signal from interference and noise. The correlator 830 may be a digital correlator with which the light intensity autocorrelation function is calculated. The scattered light of multiple angles is received by the scattered light receiving device 30, weak signals are identified and extracted by the photomultiplier 820, and enter the correlator 830 to obtain the light intensity autocorrelation function at the measured angle. The correlator 830 is connected to a computer. And the computer and related software are used for calculating the particle size distribution of the nano particles in the nano particle suspension to be measured according to the received scattered light and the recorded information of the change of the light intensity along with time. And performing inversion calculation on the particle size of the nano particles to obtain a weight coefficient ratio with the minimum error, and outputting a particle size measurement result.

In one embodiment, each of the scattered light receiving devices 30 further comprises a second goldenms prism 350 and a second prism adjustment structure 360. The second gram thomson prism 350 is disposed on the second prism adjustment structure 360. The position of the second gram thomson prism 350 is adjusted by the second prism adjustment structure 360 so that the scattered light beam is incident to the reflecting mirror 310 through the second gram thomson prism 350.

The second prism adjustment structure 360 has the same structure as the first prism adjustment structure 220.

The second prism adjusting structure 360 includes a supporting base, an adjusting table, and an adjusting shaft. The adjusting platform is arranged on the supporting seat, and the adjusting shaft is connected with the adjusting platform in a sliding mode. The second grammes prism 350 is disposed on the adjusting stage of the second prism adjusting structure 360, and the position of the adjusting stage is set by an adjusting shaft, so that the emergent light (scattered light beam) is irradiated onto the reflecting mirror 310 through the second grammes prism 350. Reflected by the mirror 310 to the fiber focus lens 320.

Specifically, each of the scattered light receiving devices 30 further includes a fixing base 370. The fixing base 370 is detachably connected to the supporting base 810. The reflector 310, the fiber focus lens 320, the optical fiber 330, the second gram thomson prism 350, and the second prism adjustment structure 360 are disposed on a fixing base 370. The fixing base 370 includes a plurality of fixing plates, which surround to form a second prism adjusting structure seating space, a mirror seating space, and a fiber focus lens seating space. The reflector placing space and the optical fiber focusing lens placing space are arranged on one side and are separated from the second prism adjusting structure placing space through the partition board. The spacer is provided with spacer plate holes 340. The mirror receiving space is used to receive the mirror 310. The optical fiber focusing lens placing space is arranged above the reflector placing space, and the optical fiber focusing lens placing space is communicated with the reflector placing space. The second prism adjustment structure installation space is used for placing the second prism adjustment structure 360. The scattered beam passes through the second gram thomson prism 350 to the spacer plate aperture 340. And, the light is irradiated to the reflecting mirror 310 through the spacer hole 340. The scattered light beam is reflected by the reflecting mirror 310 to the fiber focus lens 320, and an optical path of the scattered light beam is formed.

When the particle size of the rod-shaped nanoparticles at a certain measurement receiving angle is tested, the second gram-Thompson prism 350(Glan-Thompson) is placed on the scattered light beam receiving path to filter out the vertically polarized light in the scattered signal. At this time, the scattered light beam passes through the second gram thomson prism 350 and then is irradiated to the reflecting mirror 310 through the isolation plate hole 340.

When the spherical nanoparticle size at a certain measured acceptance angle is tested, the second gram Thompson prism 350(Glan-Thompson) is removed.

Referring to fig. 1, in one embodiment, the nanoparticle size measurement system 100 further includes a ccd camera 40. The ccd camera 40 is disposed opposite to the first placing hole 141, and is configured to record image information of the incident light beam and the scattered light beam converged at the scattering center of the sample cell 180 in real time.

Wherein the first placing hole 141 corresponds to an opening of the sample cell 180. The ccd camera 40 is disposed opposite the opening of the sample cell 180. The ccd camera 40 is connected to a computer for transmitting image information collected by the ccd camera 40. The ccd camera 40 faces the opening of the sample cell 180, and can record and display image information of incident light and emergent light (scattered light) converged at the center of the sample cell 180 in real time. Moreover, by the focusing function of the ccd camera 40, it is possible to visually observe whether the scattered light receiving optical paths of the multiple scattered light receiving devices 30 are strictly intersected with the same scattering center point of the sample cell 180, and to perform fine adjustment of the three-axis coordinates of the space to realize true concentricity. The CCD camera 40 can observe and calculate the measurement angle of the received light of the scattered light, and the accuracy of each scattered light receiving angle is ensured. Meanwhile, according to the image information collected by the ccd camera 40, the angles of the plurality of scattered light receiving devices 30 may be adjusted to realize the scattered light measurement at a certain receiving angle.

Therefore, the ccd camera 40 can detect the receiving angles of a plurality of scattered light receiving devices 30 in real time, and adjust accordingly to ensure the accuracy of each scattered light receiving angle. Therefore, the precision of intersecting multiple scattered light receiving optical paths at the same scattering center point of the sample cell 180 can be ensured by the ccd camera 40 without completely depending on the existing processing precision.

In one embodiment, the nanoparticle size measurement system 100 further includes an instrument holder 840. The scattering generating device 10, the incident light device 20, the laser 50, the attenuator 60, the first reflector 710, the second reflector 720, the heat exchanger 80, the photomultiplier 820 and the correlator 830 are detachably disposed on the instrument fixing plate 840, so that the device is convenient to detach and connect, and the portability and stability of the device are improved. Scattered light receiving arrangement 30 lens 730 set up in on the supporting seat 810, the supporting seat 810 can be dismantled and set up on the instrument fixing plate 840, conveniently dismantle the connection, improved the portability and the stability of device.

All devices in the nanoparticle size measuring system 100 can be integrated together through the instrument fixing plate 840, and the device is convenient to carry and move. The ccd camera 40 is fixed to the instrument fixing plate 840 by a plurality of camera support stands 410. And the ccd camera 40 is disposed right above the center of the sample cell 180, and is connected to a computer for recording image information of the incident light beam and the scattered light beam converged at the scattering center of the sample cell 180 in real time.

Referring to fig. 8-9, in one embodiment, the nanoparticle size measurement system 100 further includes a plurality of third placement holes 143. The plurality of third placing holes 143 are disposed in the end cap 140, and are used for placing a temperature sensor to monitor the temperature in the second receiving space 152 in real time. The nanoparticle size measurement system 100 further includes a temperature control module 191 and a plurality of temperature control structures 190. The temperature control module 191 is connected to the temperature sensor, and is configured to obtain the temperature in the second receiving space 152. The plurality of temperature control structures 190 are disposed on the outer wall of the first annular side plate 130 far away from the first receiving space 132, and the plurality of temperature control structures 190 are connected to the temperature control module 191. The temperature control module 191 adjusts and controls the plurality of temperature control structures 190 according to the temperature change in the second receiving space 152, so as to stabilize the temperature in the second receiving space 152.

The temperature control structure 190 may be disposed on the outer wall of the first annular side plate 130 at two opposite sides of the sample cell 180, so as to control temperature control. The temperature of the second receiving space 152 can be adjusted to about 80 ℃ by the temperature control structure 190. The temperature control structure 190 may be a refrigerating sheet, and the temperature is controlled by connecting a water pipe using a water circulation system.

The temperature control structure 190 is further connected with a temperature control module 191. When the temperature sensors disposed in the third placing hole 143 monitor that the temperatures in the sample cell 180 and the matching cell 150 are changed, temperature parameters are transmitted to the temperature control module 191. At this time, the temperature control structure 190 is adjusted by the temperature control module 191 to achieve stable temperature balance.

In one embodiment, the temperature control structure 190 is a circulation water pipeline, and the temperature control module 191 is connected with a circulation pump. When the temperature control module 191 monitors the temperature change in the second storage space 152 in real time, the temperature control module 191 controls the power of the circulating water pump, and then controls the water flow output of the circulating water pump, thereby realizing the temperature regulation and control. Furthermore, the temperature in the second receiving space 152 is maintained at about 80 ℃ by heat transfer, so that a stable environment is provided for the sample cell 180, and the measurement accuracy of the nanoparticle size measurement system 100 is improved.

In one embodiment, the end cap 140 is provided with two third placing holes 143. One temperature sensor is placed in one of the third placing holes 143, and one temperature sensor is placed in the sample cell 180 for monitoring the temperature in the sample cell 180. A temperature sensor is placed in the other third placing hole 143, and the temperature sensor is placed in the second receiving space 152 of the matching tank 150 for monitoring the temperature in the matching tank 150. The temperature control module 191 simultaneously monitors the temperature change in the sample cell 180 and the second receiving space 152. When the temperature control module 191 monitors that the temperature of the sample cell 180 changes, the temperature control module 191 adjusts through the temperature control structure 190, so that the temperature in the second receiving space 152 is maintained at about 80 ℃ through heat transfer, and the temperature in the sample cell 180 is maintained at about 80 ℃, thereby providing a stable environment.

Therefore, the temperature change at each position in the sample cell 180 can be made the same as a whole by the heat transfer among the temperature control structure 190, the first annular side plate 130 and the matching cell 150, and the temperature change at each position in the sample cell 180 can be synchronized. At this time, when the nanoparticles in the sample cell 180 make brownian motion in the liquid, the nanoparticles are not affected by the temperature factor, so that the nanoparticles are in a relatively stable environment. Moreover, the temperature control structure 190, the first annular side plate 130 and the matching tank 150 can transfer heat to each other, so that the problem of sudden temperature rise or sudden temperature drop in the sample tank 180 can be avoided.

In one embodiment, the temperature control module 191 includes, but is not limited to, a Central Processing Unit (CPU), an embedded microcontroller Unit (MCU), an embedded microprocessor Unit (MPU), and an embedded System on Chip (SoC).

Referring to fig. 13, in one embodiment, a nanoparticle size measuring instrument 200 includes an instrument housing 90. The instrument housing 90 encloses an instrument receiving space 910. The nanoparticle size measurement system 100 is placed in the instrument accommodating space 910, so as to provide a closed dark environment for the nanoparticle size measurement system 100, and prevent other stray light from affecting.

Wherein the heat exchanger 80 is disposed on the instrument fixing plate 840 to maintain a constant ambient temperature in the instrument accommodating space 910.

The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.

The above-mentioned embodiments only express several embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present application. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the concept of the present application, which falls within the scope of protection of the present application. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A nanoparticle size measurement system, comprising:

the scattering generating device (10) is used for enabling the nano particles to be detected to scatter at various angles under the interaction;

the scattering generating device (10) comprises a first annular side plate (130), the first annular side plate (130) surrounds a first accommodating space (132) with a first opening (131), the first annular side plate (130) is provided with an incident light through hole (110) and a plurality of scattered light through holes (120), the incident light through hole (110) and the scattered light through holes (120) are arranged on the same horizontal plane, and the axis of the incident light through hole (110) and the axis of the scattered light through holes (120) intersect at the same scattering center point;

a matching reservoir (150) disposed in the first receiving space (132), the matching reservoir (150) including a second receiving space (152) formed with a second opening (151);

a sample cell (180) disposed in the second receiving space (152) for placing a sample solution, wherein an incident light beam irradiates the sample cell (180) through the incident light through hole (110) and then forms a scattered light beam through a scattering center, and the scattered light through holes (120) are used for allowing the scattered light beam to pass through;

a matching fluid (153) that is provided in the second storage space (152) and surrounds the cuvette (180), and the refractive index of the matching fluid (153) is the same as the refractive index of the wall surface of the cuvette (180);

an end cap (140) disposed to match the first opening (131), wherein the end cap (140) is provided with a first placement hole (141), and the diameter of the sample cell (180) is smaller than that of the first placement hole (141);

a first light blocking structure support part (161) disposed between the sample cell (180) and the matching cell (150), wherein the first light blocking structure support part (161) is connected with the end cap (140);

the first light blocking structure (160) is used for absorbing and reflecting the light beam after passing through the sample cell (180), the first light blocking structure (160) is arranged between the sample cell (180) and the matching cell (150), the first light blocking structure (160) is connected with the first light blocking structure supporting part (161), and the first light blocking structure (160) is arranged on a forward extension line of an incident light beam;

the second light blocking structure (170) is arranged between the sample cell (180) and the matching cell (150), the second light blocking structure (170) is connected with the end cover (140), and the second light blocking structure (170) is arranged on a reverse extension line of the scattered light beam received by the scattered light through holes (120).

2. The nanoparticle diameter measurement system according to claim 1, wherein the second light blocking structure (170) is provided with a through hole (171), axes of the through hole (171), the incident light through hole (110) and the scattered light through holes (120) intersect at a same scattering center point, and an angle between the axis of the through hole (171) and the axis of the incident light through hole (110) at the scattering center point is 90 °.

3. The nanoparticle size measurement system of claim 1, further comprising:

an incident light device (20) for adjusting an incident light beam to enter the scattering generation device (10) through the incident light through hole (110);

the incident light device (20) comprises a first gram Thomson prism (210) and a first prism adjusting structure (220), the first gram Thomson prism (210) being arranged at the first prism adjusting structure (220);

adjusting a position of the first Glan Thomson prism (210) by the first prism adjustment structure (220) such that an incident light beam is incident to the incident light through hole (110) through the first Glan Thomson prism (210).

4. The nanoparticle size measurement system of claim 1, further comprising:

a plurality of scattered light receiving devices (30), wherein each scattered light receiving device (30) corresponds to one scattered light through hole (120) and is used for receiving scattered light beams emitted by the scattered light through holes (120);

the receiving light paths of the scattered light receiving devices (30) intersect at the same scattering center point of the sample cell (180).

5. The nanoparticle diameter measurement system according to claim 4, wherein each of the scattered light receiving devices (30) includes:

the reflecting mirror (310), one reflecting mirror (310) corresponds to one scattered light through hole (120), the reflecting mirror (310) is arranged on the light path of the scattered light beam emitted by the scattered light through hole (120) and is used for enabling the scattered light beam to be reflected at an incidence angle of 45 degrees;

the optical fiber focusing lens (320) is arranged on a scattered light beam light path reflected by the reflecting mirror (310) and is used for focusing the scattered light beam;

and the optical fiber (330) is connected with the optical fiber focusing lens (320) and is used for transmitting the scattered light beam received by the optical fiber focusing lens (320) to the photon counter through the optical fiber.

6. The nanoparticle diameter measurement system according to claim 5, wherein each of the scattered light receiving devices (30) further comprises a second grand Thomson prism (350) and a second prism adjustment structure (360);

the second Glan-Thomson prism (350) is arranged at the second prism adjustment structure (360);

adjusting a position of the second granthomson prism (350) by the second prism adjustment structure (360) so that the scattered light beam is incident to the reflecting mirror (310) through the second granthomson prism (350).

7. The nanoparticle size measurement system of claim 1, further comprising:

and the CCD camera (40) is arranged opposite to the first placing hole (141) and is used for recording image information of the incident light beams and the scattered light beams converged at the scattering central point of the sample cell (180) in real time.

8. The nanoparticle size measurement system of claim 1, further comprising:

and a plurality of third placement holes (143) provided in the end cap (140) for placing a temperature sensor to monitor the temperature in the second receiving space (152) in real time.

9. The nanoparticle size measurement system of claim 8, further comprising:

the temperature control module (191) is connected with the temperature sensor and used for acquiring the temperature in the second accommodating space (152);

the plurality of temperature control structures (190) are arranged on the outer wall of the first annular side plate (130) far away from the first accommodating space (132), and the plurality of temperature control structures (190) are connected with the temperature control module (191);

the temperature control module (191) regulates and controls the plurality of temperature control structures (190) according to the temperature change in the second receiving space (152) so as to stabilize the temperature in the second receiving space (152).

10. The nanoparticle diameter measurement system according to claim 1, wherein the end cap (140) is provided with a plurality of second placement holes (142) for placing a matching fluid pipe to convey the matching fluid (153).

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