CN101294847A - Preparation method of integrating sphere for laser power measurement - Google Patents
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- 238000005259 measurement Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 59
- 238000000034 method Methods 0.000 claims abstract description 39
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 30
- 239000001301 oxygen Substances 0.000 claims abstract description 30
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000000151 deposition Methods 0.000 claims abstract description 10
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 230000003647 oxidation Effects 0.000 claims description 20
- 238000007254 oxidation reaction Methods 0.000 claims description 20
- 239000000377 silicon dioxide Substances 0.000 claims description 17
- 239000011248 coating agent Substances 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 15
- 230000007062 hydrolysis Effects 0.000 claims description 12
- 238000006460 hydrolysis reaction Methods 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims 3
- 230000008021 deposition Effects 0.000 claims 3
- 239000004411 aluminium Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 11
- 229910052814 silicon oxide Inorganic materials 0.000 abstract 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000011863 silicon-based powder Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 description 9
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 6
- 238000001514 detection method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明主要涉及一种光探测用积分球制备方法，特别是支持激光功率测量用光探测器件的激光功率测量用积分球制备方法。The invention mainly relates to a method for preparing an integrating sphere for light detection, in particular to a method for preparing an integrating sphere for laser power measurement supporting a photodetection device for laser power measurement.
背景技术 Background technique
在现代光学测量中，广泛使用测光积分球，像光学材料的反射比测量，大都采用积分球法。积分球又称为光通球，是一个中空的完整球壳。内壁涂白色漫反射层，且球内壁各点漫射均匀。积分球的优点在于它不仅能收集样品上的全部反射光，而且球壁各部分向接收器反射的光具有对称性，与反射的角分布无关，这种性能与球的结构以及内涂层密切相关。根据测光积分球的基本原理，一束光通量由入口进入积分球后，经球内壁多次漫反射之后，到达任一窗口的光照度都是多次漫反射的积分。In modern optical measurement, the photometric integrating sphere is widely used, and the reflectance measurement of optical materials mostly adopts the integrating sphere method. Integrating sphere, also known as luminous flux sphere, is a hollow complete spherical shell. The inner wall is coated with a white diffuse reflection layer, and each point on the inner wall of the ball diffuses evenly. The advantage of the integrating sphere is that it can not only collect all the reflected light on the sample, but also the light reflected from each part of the sphere wall to the receiver has symmetry, which has nothing to do with the angular distribution of reflection. This performance is closely related to the structure of the sphere and the inner coating. relevant. According to the basic principle of the photometric integrating sphere, after a beam of luminous flux enters the integrating sphere from the entrance, after multiple diffuse reflections on the inner wall of the sphere, the illuminance reaching any window is the integral of multiple diffuse reflections.
对于现有积分球光功率计，其主要有两个制备方法，分别是采用聚四氟乙烯模压法制备和硫酸钡喷涂法。采用聚四氟乙烯模压法制备的积分球漫反射性能好，但价格昂贵。我国照明业长期以来存在这样的误区：积分球内涂层越白越好，即反射率越高越好。事实上很白的积分球内涂层(通常为硫酸钡涂层)，不仅反射率变化较大，易脏，粘结剂使用不当易返黄，而且光谱反射率不平坦，主要是短波蓝光部分下跌较大，对测光精确度影响较大，并且硫酸钡涂层牢固性不佳，容易脱落，这将直接导致测量结果的不准确。For the existing integrating sphere optical power meter, there are mainly two preparation methods, which are respectively adopting polytetrafluoroethylene molding method and barium sulfate spraying method. Integrating spheres prepared by polytetrafluoroethylene molding method have good diffuse reflection performance, but are expensive. There has been such a misunderstanding in my country's lighting industry for a long time: the whiter the inner coating of the integrating sphere, the better, that is, the higher the reflectivity, the better. In fact, the inner coating of a very white integrating sphere (usually barium sulfate coating) not only has a large change in reflectance, is easy to get dirty, and is easy to return to yellow if the binder is used improperly, but also has an uneven spectral reflectance, mainly short-wave blue light. A large drop will have a great impact on the photometric accuracy, and the barium sulfate coating is not firm enough to fall off easily, which will directly lead to inaccurate measurement results.
因此，我们提出了利用氧化烧结二氧化硅涂层的方法制备积分球光功率计的漫反射层，由于工艺步骤采用喷涂法产生二氧化硅粉末层，因此制备工艺简单；由于采用高温烧结，膜层结构致密，附着质量好。这种方法在保证积分球漫反射特性的前提下工艺相对简单，在国际上还没有报道。Therefore, we proposed to use the method of oxidizing and sintering silica coating to prepare the diffuse reflection layer of the integrating sphere optical power meter. Since the process steps adopt the spraying method to produce the silica powder layer, the preparation process is simple; due to the high temperature sintering, the film The layer structure is dense and the adhesion quality is good. This method has a relatively simple process under the premise of ensuring the diffuse reflection characteristics of the integrating sphere, and has not been reported internationally.
发明内容 Contents of the invention
本发明的目的在于提供了一种光探测用积分球制备方法，其是采用火焰水解法沉积二氧化硅粉末，方法简单，制备成本低，因其采用高温氧化烧结方式制备二氧化硅膜层，结构致密，附着性能好；采用沉积方法，对积分球设计尺寸无要求，提高适用性。The purpose of the present invention is to provide a method for preparing an integrating sphere for optical detection, which uses a flame hydrolysis method to deposit silicon dioxide powder. The method is simple and the preparation cost is low, because the silicon dioxide film layer is prepared by high-temperature oxidation and sintering. The structure is dense and the adhesion performance is good; the deposition method is adopted, and there is no requirement for the design size of the integrating sphere, which improves the applicability.
本发明提供一种激光功率测量用积分球制备方法，其特征在于，包括如下步骤：The invention provides a method for preparing an integrating sphere for laser power measurement, which is characterized in that it comprises the following steps:
步骤1：取一金属球，该金属球为中空结构；Step 1: Take a metal ball, which is a hollow structure;
步骤2：在金属球中空形腔体内表面沉积一层二氧化硅粉末层；Step 2: Deposit a layer of silicon dioxide powder on the inner surface of the hollow cavity of the metal ball;
步骤3：对二氧化硅粉末层进行湿氧、干氧交替氧化，使二氧化硅粉末层烧结为均匀致密的白色二氧化硅膜层。Step 3: alternately oxidize the silicon dioxide powder layer with wet oxygen and dry oxygen, so that the silicon dioxide powder layer is sintered into a uniform and dense white silicon dioxide film layer.
其中步骤1所说的金属球的材料为铁或铝或铜。Wherein the material of said metal ball in step 1 is iron or aluminum or copper.
其中步骤2所说的在金属球形腔体内表面沉积一层二氧化硅粉末层的方法是火焰水解方法。Wherein the method of depositing a layer of silicon dioxide powder layer on the inner surface of the metal spherical cavity mentioned in step 2 is a flame hydrolysis method.
其中所说的通过火焰水解方法沉积一层二氧化硅粉末层时，在反应气体中加入磷、硼元素以调节氧化温度。Wherein, when depositing a layer of silicon dioxide powder layer by flame hydrolysis method, phosphorus and boron elements are added to the reaction gas to adjust the oxidation temperature.
其中步骤3所说的湿氧、干氧交替氧化，在氧化过程中是通过调节氧气流量改变二氧化硅膜层致密度。Wherein the wet oxygen and dry oxygen alternate oxidation mentioned in step 3 is to change the density of the silicon dioxide film layer by adjusting the oxygen flow rate during the oxidation process.
其中步骤3所说的对二氧化硅粉末层进行湿氧、干氧交替氧化，该交替氧化的次数为2-5次。Wherein step 3 said that the silicon dioxide powder layer is alternately oxidized with wet oxygen and dry oxygen, and the number of times of the alternate oxidation is 2-5 times.
其中所说的湿氧、干氧交替氧化的氧化温度为800至1100摄氏度。The oxidation temperature of said wet oxygen and dry oxygen alternate oxidation is 800 to 1100 degrees centigrade.
本发明提供的一种光探测用积分球制备方法，其具有以下优点：A method for preparing an integrating sphere for photodetection provided by the invention has the following advantages:
1、采用火焰水解法沉积二氧化硅粉末，方法简单，制备成本低。1. The silica powder is deposited by the flame hydrolysis method, which is simple and low in preparation cost.
2、采用高温氧化烧结方式制备二氧化硅膜层，结构致密，附着性能好。2. The silicon dioxide film layer is prepared by high-temperature oxidation and sintering, which has a dense structure and good adhesion.
3、采用沉积方法，对积分球设计尺寸无要求，提高适用性。3. Using the deposition method, there is no requirement for the design size of the integrating sphere, which improves the applicability.
附图说明 Description of drawings
为了进一步说明本发明的特征和效果，下面结合附图和实施例对本发明做进一步的说明，其中：In order to further illustrate the features and effects of the present invention, the present invention will be further described below in conjunction with the accompanying drawings and embodiments, wherein:
图1为光探测用积分球结构示意图；Fig. 1 is the schematic diagram of the structure of an integrating sphere for light detection;
图2为积分球腔体内壁通过火焰水解法喷涂二氧化硅粉末及烧结成膜工艺流程图。Fig. 2 is a process flow chart of spraying silicon dioxide powder on the inner wall of the cavity of the integrating sphere by flame hydrolysis and sintering to form a film.
具体实施方式 Detailed ways
请参阅图1和图2所示，本发明一种激光功率测量用积分球制备方法，包括如下步骤：Please refer to Fig. 1 and shown in Fig. 2, a kind of laser power measurement integrating sphere preparation method of the present invention comprises the following steps:
步骤1：取一金属球10，该金属球10为中空结构；该金属球10的材料为铁或铝或铜；Step 1: Take a metal ball 10, the metal ball 10 is a hollow structure; the material of the metal ball 10 is iron or aluminum or copper;
步骤2：在金属球10中空形腔体内表面沉积一层二氧化硅粉末层40；所说的在金属球10形腔体内表面沉积一层二氧化硅粉末层40的方法是火焰水解方法；采用火焰水解方法沉积二氧化硅粉末层40时，在反应气体中加入磷、硼元素以调节氧化温度；Step 2: Deposit a layer of silicon dioxide powder layer 40 on the inner surface of the hollow cavity of the metal ball 10; the method of depositing a layer of silicon dioxide powder layer 40 on the inner surface of the metal ball 10-shaped cavity is a flame hydrolysis method; When the silicon dioxide powder layer 40 is deposited by the flame hydrolysis method, phosphorus and boron elements are added to the reaction gas to adjust the oxidation temperature;
步骤3：对二氧化硅粉末层40进行湿氧、干氧交替氧化，使二氧化硅粉末层40烧结为均匀致密的白色二氧化硅膜层；所说的湿氧、干氧交替氧化，在氧化过程中是通过调节氧气流量改变二氧化硅膜层致密度；所说的对二氧化硅粉末层40进行湿氧、干氧交替氧化，该交替氧化的次数为2-5次；其中所说的湿氧、干氧交替氧化的氧化温度为800至1100摄氏度。Step 3: alternately oxidize the silicon dioxide powder layer 40 with wet oxygen and dry oxygen, so that the silicon dioxide powder layer 40 is sintered into a uniform and dense white silicon dioxide film layer; In the oxidation process, the density of the silicon dioxide film layer is changed by adjusting the flow rate of oxygen; said silicon dioxide powder layer 40 is alternately oxidized with wet oxygen and dry oxygen, and the number of times of the alternate oxidation is 2-5 times; wherein said The oxidation temperature of wet oxygen and dry oxygen alternate oxidation is 800 to 1100 degrees Celsius.
其再参阅图1，图1是描述光探测用积分球结构示意图。该器件包括积分金属球10，该金属球10有一中空腔体；在金属球10上开有入射孔20，该入射孔20用于激光入射；在金属球10上开有圆孔30，该圆孔30用于安装光电探测器，该入射孔20与圆孔30相差90度；在金属球10的内表面附着一层通过火焰水解法沉积并经过干湿氧氧化烧结的二氧化硅粉末层40，该二氧化硅粉末层40为二氧化硅膜层；烧结的二氧化硅膜层主要作用是将入射光均匀的漫反射到积分球内，以减少探测器对入射光几何尺寸及偏振态的影响；积分球内壁挡板50的作用是避免入射光线在未经过漫反射的条件下直接经开孔30照射到光电探测器上，防止接收器直接接收第一次反射光，只接收积分光，从而提高测量准确度。Referring to FIG. 1 again, FIG. 1 is a schematic diagram describing the structure of an integrating sphere for light detection. The device includes an integrating metal ball 10, the metal ball 10 has a hollow cavity; an incident hole 20 is opened on the metal ball 10, and the incident hole 20 is used for laser incident; a circular hole 30 is opened on the metal ball 10, the circle The hole 30 is used to install a photodetector, and the incident hole 20 is 90 degrees different from the circular hole 30; a layer of silicon dioxide powder layer 40 deposited by flame hydrolysis and sintered by dry and wet oxygen oxidation is attached to the inner surface of the metal ball 10 , the silicon dioxide powder layer 40 is a silicon dioxide film layer; the main function of the sintered silicon dioxide film layer is to uniformly reflect the incident light into the integrating sphere, so as to reduce the detector's influence on the geometric size and polarization state of the incident light. Influence; the function of the baffle plate 50 on the inner wall of the integrating sphere is to prevent the incident light from directly irradiating the photodetector through the opening 30 without diffuse reflection, so as to prevent the receiver from directly receiving the reflected light for the first time and only receive the integrated light. Thereby improving measurement accuracy.
请再参阅图2，图2是描述积分球腔体内壁通过火焰水解法沉积二氧化硅粉末工艺示意图。首先在积分球内壁通过火焰水解法沉积一层二氧化硅粉末，若一次喷涂粉末厚度不足，可通过扫描方式反复沉积直到二氧化硅粉末层达到要求厚度；然后将积分球放入通有干湿氧的氧化炉中进行烧结，烧结温度为800摄氏度至1100摄氏度，烧结过程中可以通过干湿氧氛围的交替以及改变烧结温度，调节烧结后的二氧化硅膜层致密度。Please refer to FIG. 2 again. FIG. 2 is a schematic diagram describing the process of depositing silicon dioxide powder on the inner wall of the cavity of the integrating sphere by flame hydrolysis. First, a layer of silicon dioxide powder is deposited on the inner wall of the integrating sphere by flame hydrolysis. If the thickness of the powder sprayed at one time is not enough, it can be deposited repeatedly by scanning until the silicon dioxide powder layer reaches the required thickness; Sintering is carried out in an oxygen oxidation furnace, and the sintering temperature is 800 degrees Celsius to 1100 degrees Celsius. During the sintering process, the density of the sintered silicon dioxide film layer can be adjusted by alternating dry and wet oxygen atmospheres and changing the sintering temperature.
我们研制的新型测光积分球，是用二氧化硅粉末烧结涂层代替常用的氧化镁(MgO)、硫酸钡(BaSO4)作积分球涂层，在光通信用波长范围内，光谱反射比较高，且反射比中性好，有利于减小它对积分球非中性的影响。The new photometric integrating sphere developed by us uses silica powder sintered coating instead of commonly used magnesium oxide (MgO) and barium sulfate (BaSO 4 ) as the integrating sphere coating. In the wavelength range for optical communication, the spectral reflection is relatively High, and the reflectance is better than neutral, which is beneficial to reduce its influence on the non-neutrality of the integrating sphere.
新型二氧化硅粉末烧结涂层积分球由于其反射比较高，因此可以大大提高积分球的效率，这有利于低透射、弱反射光信号测量，不仅可以提高测量的灵敏度，而且也大大改善了测量的信噪比.The new silica powder sintered coating integrating sphere can greatly improve the efficiency of the integrating sphere due to its high reflection ratio, which is beneficial to the measurement of light signals with low transmission and weak reflection, not only can improve the sensitivity of the measurement, but also greatly improve the measurement signal-to-noise ratio.
另外，由于涂层采用烧结制备，涂层粘性好，不易破裂与起皱，灰尘可以用清洁的毛刷清除，不会损伤涂层。二氧化硅粉末烧结涂层不怕潮湿，暴露在紫外光下也不会变黄，具有很好的环境适应性，能够广泛应用与实验室外的实际生产环境中。In addition, because the coating is prepared by sintering, the coating has good viscosity, is not easy to crack and wrinkle, and the dust can be removed with a clean brush without damaging the coating. Silica powder sintered coating is not afraid of moisture and will not turn yellow when exposed to ultraviolet light. It has good environmental adaptability and can be widely used in actual production environments outside the laboratory.
由于温度对测量具有一定的影响，为了进一步增加测量的准确性，可在积分球内增加温度传感装置，记录测量时实际温度，通过温度控制或者计算补偿等方式进行修正，从而实现高精度测量。Since the temperature has a certain influence on the measurement, in order to further increase the accuracy of the measurement, a temperature sensing device can be added in the integrating sphere to record the actual temperature during the measurement, and correct it by means of temperature control or calculation compensation to achieve high-precision measurement .
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102410875A (en) * | 2011-08-15 | 2012-04-11 | 西北核技术研究所 | Array attenuator of high-energy laser and manufacturing method thereof |
| CN102707212A (en) * | 2011-10-28 | 2012-10-03 | 杭州浙大三色仪器有限公司 | Device for detecting service life of light emitting diode (LED) in real time |
| CN105675128A (en) * | 2016-01-25 | 2016-06-15 | 武汉浩宏科技有限公司 | Laser energy detector |
| CN109580172A (en) * | 2018-11-06 | 2019-04-05 | 中国计量科学研究院 | A kind of micro-imaging radiometric calibration substrate and preparation method thereof |
| CN111867730A (en) * | 2018-03-14 | 2020-10-30 | 格兰森斯股份公司 | Sample container and tool for use in an integrating chamber |
| CN115198373A (en) * | 2022-07-22 | 2022-10-18 | 安徽易芯半导体有限公司 | Device and method for growing silicon dioxide film by thermal oxidation method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3702775A (en) * | 1971-02-12 | 1972-11-14 | Nasa | Diffuse reflective coating |
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2007
- 2007-04-28 CN CN200710097692A patent/CN100575895C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102410875A (en) * | 2011-08-15 | 2012-04-11 | 西北核技术研究所 | Array attenuator of high-energy laser and manufacturing method thereof |
| CN102707212A (en) * | 2011-10-28 | 2012-10-03 | 杭州浙大三色仪器有限公司 | Device for detecting service life of light emitting diode (LED) in real time |
| CN105675128A (en) * | 2016-01-25 | 2016-06-15 | 武汉浩宏科技有限公司 | Laser energy detector |
| CN111867730A (en) * | 2018-03-14 | 2020-10-30 | 格兰森斯股份公司 | Sample container and tool for use in an integrating chamber |
| US11975331B2 (en) | 2018-03-14 | 2024-05-07 | Grainsense Oy | Sample containers for use inside integrating cavities, and tools |
| CN109580172A (en) * | 2018-11-06 | 2019-04-05 | 中国计量科学研究院 | A kind of micro-imaging radiometric calibration substrate and preparation method thereof |
| CN115198373A (en) * | 2022-07-22 | 2022-10-18 | 安徽易芯半导体有限公司 | Device and method for growing silicon dioxide film by thermal oxidation method |
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|---|---|
| CN100575895C (en) | 2009-12-30 |
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