CN105296960A - Preparation method of homogenized boron nitride coating - Google Patents
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- 238000000576 coating method Methods 0.000 title claims abstract description 45
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 44
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000011248 coating agent Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000151 deposition Methods 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 32
- 230000008021 deposition Effects 0.000 claims abstract description 31
- 239000007789 gas Substances 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 14
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000012159 carrier gas Substances 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 239000003085 diluting agent Substances 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000007669 thermal treatment Methods 0.000 claims 1
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 13
- 239000002131 composite material Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 239000012495 reaction gas Substances 0.000 abstract description 3
- 230000005641 tunneling Effects 0.000 abstract description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 abstract 1
- 238000001514 detection method Methods 0.000 abstract 1
- 238000007740 vapor deposition Methods 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 6
- 229910010271 silicon carbide Inorganic materials 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910015900 BF3 Inorganic materials 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012783 reinforcing fiber Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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Abstract
本发明涉及一种均匀化氮化硼涂层的制备方法。给方法以三氯化硼（BCl3）和氨气（NH3）为反应气体，通入反应器中，先在混合区混合均匀，再在沉积反应区发生表面沉积，最后将所得样品进行高温热处理，经扫描隧道显微镜（SEM）、傅立叶红外（FT-IR）和X射线衍射（XRD）检测，制备出厚度均匀、成分单一、结晶度较高的氮化硼涂层。此方法可用于复合材料中氮化硼界面的制备其它样品表面氮化硼涂层的制备，还可用于研究氮化硼气相沉积过程及机理的研究。该方法主要解决的是双组元化学气相沉积氮化硼过程中气体混合不均的问题，以提高氮化硼涂层的均匀度，更好地控制涂层厚度。
The invention relates to a method for preparing a uniform boron nitride coating. The method uses boron trichloride (BCl 3 ) and ammonia gas (NH 3 ) as the reaction gas, which are passed into the reactor, first mixed uniformly in the mixing zone, and then surface deposition occurs in the deposition reaction zone, and finally the obtained sample is subjected to high temperature After heat treatment, scanning tunneling microscope (SEM), Fourier transform infrared (FT-IR) and X-ray diffraction (XRD) detection, a boron nitride coating with uniform thickness, single composition and high crystallinity was prepared. This method can be used for the preparation of boron nitride interface in composite materials, the preparation of boron nitride coating on the surface of other samples, and can also be used to study the process and mechanism of boron nitride vapor deposition. The method mainly solves the problem of uneven gas mixing in the process of bicomponent chemical vapor deposition of boron nitride, so as to improve the uniformity of the boron nitride coating and better control the coating thickness.
Description
技术领域 technical field
本发明涉及一种化学气相沉积技术制备均匀化氮化硼涂层的方法，尤其涉及一种纤维、纤维编织件及复合材料中氮化硼界面的制备。 The invention relates to a method for preparing a homogenized boron nitride coating by chemical vapor deposition technology, in particular to the preparation of a boron nitride interface in fibers, fiber braids and composite materials.
背景技术 Background technique
氮化硼界面可以通过在复合材料制备过程中原位生成，也可以在纤维表面首先制备出界面，再将带有氮化硼界面的纤维作为增强纤维应用到复合材料中，采用何种方法制取，这取决于生产工艺条件的控制及生产设备的局限性。目前，制备BN界面的方法有很多种，主要包括液相法（也称为浸渍-涂覆法）、化学气相沉积法和碳热还原法。在众多制备方法中，尤以CVD法所制得的界面性能更为优异且稳定。CVD法对设备的要求高，影响界面性能的工艺参数较多，但所得的涂层的质量往往较高，是制备高质量界面材料的首选。 The boron nitride interface can be generated in situ during the preparation of the composite material, or the interface can be prepared on the surface of the fiber first, and then the fiber with the boron nitride interface can be applied to the composite material as a reinforcing fiber, and what method is used to prepare it , which depends on the control of production process conditions and the limitations of production equipment. At present, there are many methods for preparing BN interfaces, mainly including liquid phase method (also known as dipping-coating method), chemical vapor deposition method and carbothermal reduction method. Among many preparation methods, the interface properties prepared by CVD method are more excellent and stable. The CVD method has high requirements on equipment, and there are many process parameters that affect the interface performance, but the quality of the obtained coating is often high, so it is the first choice for preparing high-quality interface materials.
采用CVD法制备氮化硼涂层中，主要采用BX3+NH3双组元系统，其中应用最多的为BCl3+NH3系统，但是，与单组元系统相比，由于沉积系统处于高温低压状态下，源气体反应剧烈，气体混合不均，导致不同位置气体浓度不同，沉积速率不同，继而造成沉积基底表面的涂层厚度、涂层晶粒大小及涂层结晶度不同，不利于基底表面生成厚度均匀、成分单一、结晶度较高的氮化硼涂层。相关文献及专利中指出，化学气相法制备氮化硼涂层过程中，均采用直接在恒温区沉积的方法，双组元气体在沉积区相遇并发生化学反应，继而在基底表面沉积氮化硼涂层，对所得涂层进行表征，发现沉积不均现象。此专利中指出，通过先混合再沉积的方法，可以有效地解决这一问题，获得相对稳定、均匀的氮化硼涂层。 In the preparation of boron nitride coating by CVD method, the BX 3 +NH 3 two-component system is mainly used, and the most widely used is the BCl 3 +NH 3 system. However, compared with the single-component system, since the deposition system is at a high temperature Under low pressure, the source gas reacts violently and the gas mixes unevenly, resulting in different gas concentrations and different deposition rates at different positions, which in turn causes differences in the coating thickness, coating grain size and coating crystallinity on the surface of the deposited substrate, which is not conducive to the substrate. A boron nitride coating with uniform thickness, single composition and high crystallinity is formed on the surface. Relevant literature and patents pointed out that in the process of preparing boron nitride coating by chemical vapor phase method, the method of direct deposition in the constant temperature zone is adopted. The two-component gas meets and reacts chemically in the deposition zone, and then deposits boron nitride on the surface of the substrate. Coatings, the resulting coatings were characterized and non-uniform deposition was found. It is pointed out in this patent that this problem can be effectively solved by mixing first and then depositing, and a relatively stable and uniform boron nitride coating can be obtained.
发明内容：Invention content:
本发明的目的是提供一种双组元气体化学气相沉积法制备氮化硼涂层的方法，用于解决现有技术的缺陷和不足，提供一种制备均匀涂层的方法，尤其是一种采用BX3+NH3体系化学气相沉积法制备氮化硼涂层的方法。 The purpose of the present invention is to provide a method for preparing a boron nitride coating by a two-component gas chemical vapor deposition method, which is used to solve the defects and deficiencies of the prior art, and provides a method for preparing a uniform coating, especially a The invention discloses a method for preparing a boron nitride coating by adopting a BX 3 +NH 3 system chemical vapor deposition method.
本方法对常用的化学气相沉积法进行了优化，通过先混合再沉积的方法，解决氮化硼涂层不均匀的问题，获得相对均匀、成分单一、结晶性能良好的氮化硼涂层。本发明所用的技术方案主要包括：气体混合、化学气相沉积和高温热处理。 The method optimizes the commonly used chemical vapor deposition method, solves the problem of uneven boron nitride coating by mixing first and then depositing, and obtains a relatively uniform boron nitride coating with single composition and good crystallization performance. The technical solution used in the invention mainly includes: gas mixing, chemical vapor deposition and high temperature heat treatment.
具体采用如下技术方案： Specifically, the following technical solutions are adopted:
一种均匀化氮化硼涂层的制备方法，其特征在于该方法的具体步骤为： A method for preparing a homogenized boron nitride coating, characterized in that the specific steps of the method are:
a.将待涂样品放入沉积模具中沉积区内；通入反应气体三氯化硼、氨气；三氯化硼和氨气分别由两个进气口通入，在进入模具之前不发生接触；气体在等温混合区混合均匀；混合均匀后，气体进入沉积区，在沉积温度为300~1800℃，系统压力为1~300mbar下，发生沉积，沉积时间为0.5h~20h，最后在待涂样品表面得到均匀的氮化硼涂层；所述的三氯化硼和氨气的气体流量比为[NH3]/[BCl3]=1：1～30； a. Put the sample to be coated into the deposition area of the deposition mold; pass the reaction gas boron trichloride and ammonia gas; boron trichloride and ammonia gas are respectively passed through two air inlets, and do not occur before entering the mold Contact; the gas is mixed evenly in the isothermal mixing zone; after mixing evenly, the gas enters the deposition zone, and deposition occurs at a deposition temperature of 300~1800°C and a system pressure of 1~300mbar. The deposition time is 0.5h~20h, and finally in the waiting Coating the surface of the sample to obtain a uniform boron nitride coating; the gas flow ratio of boron trichloride and ammonia gas is [NH 3 ]/[BCl 3 ]=1:1～30;
b.沉积反应结束后，对所得氮化硼涂层样品进行高温热处理，热处理温度为1200~2000℃，时间为0.5h~5h，得到六方氮化硼涂层。 b. After the deposition reaction, the obtained boron nitride coating sample is subjected to high-temperature heat treatment at a temperature of 1200-2000°C for 0.5h-5h to obtain a hexagonal boron nitride coating.
上述的反应气体中还有载气和稀释气体；所述的载气为氮气或氩气中的至少一种，该载气与三氯化硼同一进气口进入混合区，气体流量比为[载气]:[BCl3]=1:1~120；所述的稀释气体为氢气，气体流量比为[载气]:[BCl3]=1:1~100。 There are also carrier gas and dilution gas in the above-mentioned reaction gas; the carrier gas is at least one of nitrogen or argon, and the carrier gas enters the mixing zone with the same inlet of boron trichloride, and the gas flow ratio is [ Carrier gas]:[BCl 3 ]=1:1~120; the diluent gas is hydrogen, and the gas flow ratio is [carrier gas]:[BCl 3 ]=1:1~100.
所述的化学气相沉积法制备均匀氮化硼涂层的方法，其中气体的通入方式为BCl3和NH3分为两路进入反应模具，BCl3和载气一起通入，H2可通过任一进气口通入。 The method for preparing a uniform boron nitride coating by the chemical vapor deposition method, wherein the gas feeding method is that BCl 3 and NH 3 are divided into two paths and enter the reaction mold, BCl 3 and carrier gas are fed together, and H 2 can pass through Either inlet is connected.
该化学气相沉积制备均匀氮化硼涂层的方法，可用于碳纤维、陶瓷纤维及其编织件表面氮化硼涂层的制备，也可用于复合材料中氮化硼界面的制备，同时也可用于硅片、石墨及Al2O3表面氮化硼涂层的制备和其它双组元气体化学气相沉积。 The method for preparing a uniform boron nitride coating by chemical vapor deposition can be used for the preparation of boron nitride coatings on the surface of carbon fibers, ceramic fibers and their braids, and can also be used for the preparation of boron nitride interfaces in composite materials, and can also be used for Preparation of boron nitride coating on silicon wafer, graphite and Al 2 O 3 surface and chemical vapor deposition of other two-component gases.
使用本发明沉积氮化硼涂层，结果显示，通过先混合再沉积的方法，可以制备出厚度均匀、结构单一、结晶性能良好的氮化硼涂层，与以往的制备技术相比，具有以下优点：一方面，更容易控制氮化硼涂层的厚度，使得涂层成分及结构单一稳定；另一方面，在工业化过程中，对大件样品涂覆氮化硼涂层时，可以使不同位置处表面涂层更均匀；最后，对研究沉积动力学提供了一种方法。 Using the present invention to deposit boron nitride coating, the results show that by mixing first and then depositing, a boron nitride coating with uniform thickness, single structure and good crystallinity can be prepared. Compared with the previous preparation technology, it has the following advantages: Advantages: On the one hand, it is easier to control the thickness of the boron nitride coating, making the composition and structure of the coating stable; The surface coating is more uniform at the location; finally, a method for studying the deposition kinetics is provided.
附图说明 Description of drawings
图1是反应器示意图，主要分为混合区和沉积区。 Figure 1 is a schematic diagram of the reactor, which is mainly divided into a mixing zone and a deposition zone.
图2和图3是实施例1中沉积氮化硼涂层后碳化硅纤维的SEM图。 2 and 3 are SEM images of silicon carbide fibers after depositing a boron nitride coating in Example 1.
具体实施方式 detailed description
实施例1 Example 1
第一步：装炉，将碳化硅纤维放置于沉积区，混合腔和反应腔同时处于炉管恒温区，抽真空检查系统气密性。 The first step: install the furnace, place the silicon carbide fiber in the deposition area, the mixing chamber and the reaction chamber are in the constant temperature area of the furnace tube at the same time, and check the air tightness of the system by vacuuming.
第二步：排空升温，通入高纯氮气，抽真空，如此循环五次，排除系统中残余空气，按照设定程序升温。 Step 2: Evacuate and heat up, introduce high-purity nitrogen, vacuumize, and cycle like this five times to remove residual air in the system, and heat up according to the set program.
第三步：进气，升温至设定沉积温度800℃，维持系统压力20mbar，从进气口1通入氨气60ml/min，进气口2通入高纯氮气100mlmin和三氯化硼20ml/min。 Step 3: Intake air, heat up to the set deposition temperature of 800°C, maintain the system pressure at 20mbar, feed ammonia gas 60ml/min from inlet 1, and feed high-purity nitrogen 100mlmin and boron trichloride 20ml into inlet 2 /min.
第四步：混合沉积，气体进入恒温区，先经混合腔混合，再进入沉积区在碳化硅纤维表面沉积氮化硼2h。 The fourth step: mixed deposition, the gas enters the constant temperature zone, first mixed in the mixing chamber, and then enters the deposition zone to deposit boron nitride on the surface of the silicon carbide fiber for 2 hours.
第五步：热处理，将沉积后的碳化硅纤维在氩气氛围中1300℃热处理1h。 The fifth step: heat treatment, the deposited silicon carbide fiber is heat treated at 1300° C. for 1 hour in an argon atmosphere.
对实施例1中所得沉积后的碳化硅纤维进行扫描隧道显微镜（SEM）测试，发现纤维表面沉积了一层均匀光滑的氮化硼涂层，且置于沉积区内不同位置的碳化硅纤维沉积氮化硼涂层厚度基本一致，为1um左右。 A scanning tunneling microscope (SEM) test was performed on the deposited silicon carbide fibers obtained in Example 1, and it was found that a layer of uniform and smooth boron nitride coating was deposited on the surface of the fibers, and the silicon carbide fibers placed at different positions in the deposition area were deposited The thickness of the boron nitride coating is basically the same, about 1um.
实施例2 Example 2
第一步：装炉，将清洗后的石墨板放置于沉积区，混合腔和反应腔同时处于炉管恒温区，抽真空检查系统气密性。 The first step: install the furnace, place the cleaned graphite plate in the deposition area, the mixing chamber and the reaction chamber are in the constant temperature area of the furnace tube at the same time, and check the air tightness of the system by vacuuming.
第二步：排空升温，通入高纯氮气，抽真空，如此循环五次，排除系统中残余空气，按照设定程序升温。 Step 2: Evacuate and heat up, introduce high-purity nitrogen, vacuumize, and cycle like this five times to remove residual air in the system, and heat up according to the set program.
第三步：进气，升温至设定沉积温度1300℃，维持系统压力20mbar，从进气口1通入氨气60ml/min，进气口2通入高纯氮气100mlmin和三氯化硼20ml/min。 Step 3: Intake air, heat up to the set deposition temperature of 1300°C, maintain the system pressure at 20mbar, feed ammonia gas 60ml/min from inlet 1, and feed high-purity nitrogen 100mlmin and boron trichloride 20ml into inlet 2 /min.
第四步：混合沉积，气体进入恒温区，先经混合腔混合，再进入沉积区在石墨板表面沉积氮化硼5h。 The fourth step: mixed deposition, the gas enters the constant temperature zone, first mixed in the mixing chamber, and then enters the deposition zone to deposit boron nitride on the surface of the graphite plate for 5 hours.
第五步：热处理，将沉积后的石墨板在氩气氛围中1600℃热处理1h。 The fifth step: heat treatment, the deposited graphite plate is heat treated at 1600° C. for 1 hour in an argon atmosphere.
实施例3 Example 3
第一步：装炉，将针刺碳毡放置于沉积区，混合腔和反应腔同时处于炉管恒温区，抽真空检查系统气密性。 The first step: install the furnace, place the needle-punched carbon felt in the deposition area, the mixing chamber and the reaction chamber are in the constant temperature area of the furnace tube at the same time, and check the air tightness of the system by vacuuming.
第二步：排空升温，通入高纯氮气，抽真空，如此循环五次，排除系统中残余空气，按照设定程序升温。 Step 2: Evacuate and heat up, introduce high-purity nitrogen, vacuumize, and cycle like this five times to remove residual air in the system, and heat up according to the set program.
第三步：进气，升温至设定沉积温度750℃，维持系统压力20mbar，从进气口1通入氨气60ml/min和氢气100ml/min，进气口2通入高纯氮气100mlmin和三氟化硼20ml/min。 Step 3: Intake air, heat up to the set deposition temperature of 750°C, maintain the system pressure at 20mbar, feed ammonia 60ml/min and hydrogen 100ml/min from inlet 1, and feed high-purity nitrogen 100ml/min and Boron trifluoride 20ml/min.
第四步：混合沉积，气体进入恒温区，先经混合腔混合，再进入沉积区在针刺毯毡表面沉积氮化硼0.5h。 The fourth step: mixed deposition, the gas enters the constant temperature zone, first mixed in the mixing chamber, and then enters the deposition zone to deposit boron nitride on the surface of the needle felt for 0.5h.
第五步：热处理，将沉积后的针刺碳毡在氩气氛围中1400℃热处理2h。 The fifth step: heat treatment, the deposited needle-punched carbon felt is heat-treated at 1400° C. for 2 hours in an argon atmosphere.
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Cited By (9)
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|---|---|---|---|---|
| CN105842767A (en) * | 2016-05-04 | 2016-08-10 | 上海大学 | Equipment for preparing diffractive optical element by adopting microscopic pattern electrode thermal polarization and method thereof |
| CN107058975A (en) * | 2017-01-23 | 2017-08-18 | 上海大学 | Based on parameter region control high throughput chemical gas-phase permeation technique, using and device |
| CN107460447A (en) * | 2017-09-25 | 2017-12-12 | 何军舫 | A kind of production method of the boron nitride plectane with high-flatness |
| CN107863173A (en) * | 2017-11-01 | 2018-03-30 | 中国科学院合肥物质科学研究院 | High energy particle degrader part and preparation method thereof |
| CN108545914A (en) * | 2018-05-18 | 2018-09-18 | 山东国晶新材料有限公司 | A kind of preparation method of the pyrolytic boron nitride coating layer hot bending die for the anti-aliquation solving oxidation |
| CN109234703A (en) * | 2018-11-27 | 2019-01-18 | 湖南顶立科技有限公司 | A kind of gas-phase deposition system |
| CN111363544A (en) * | 2018-12-26 | 2020-07-03 | 中国科学院物理研究所 | Phosphorus-like electron-doped hexagonal boron nitride and preparation method thereof |
| CN115968361A (en) * | 2020-08-21 | 2023-04-14 | 赛峰航空陶瓷技术公司 | Method for depositing a coating on a line in a microwave field |
| CN117089825A (en) * | 2023-06-01 | 2023-11-21 | 无锡松煜科技有限公司 | Plating chamber with uniform fluid distribution and plating method |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105842767A (en) * | 2016-05-04 | 2016-08-10 | 上海大学 | Equipment for preparing diffractive optical element by adopting microscopic pattern electrode thermal polarization and method thereof |
| CN105842767B (en) * | 2016-05-04 | 2018-05-01 | 上海大学 | The device and method of diffraction optical element are prepared using micro- pattern electrode thermal poling |
| CN107058975A (en) * | 2017-01-23 | 2017-08-18 | 上海大学 | Based on parameter region control high throughput chemical gas-phase permeation technique, using and device |
| CN107460447A (en) * | 2017-09-25 | 2017-12-12 | 何军舫 | A kind of production method of the boron nitride plectane with high-flatness |
| CN107863173A (en) * | 2017-11-01 | 2018-03-30 | 中国科学院合肥物质科学研究院 | High energy particle degrader part and preparation method thereof |
| CN108545914A (en) * | 2018-05-18 | 2018-09-18 | 山东国晶新材料有限公司 | A kind of preparation method of the pyrolytic boron nitride coating layer hot bending die for the anti-aliquation solving oxidation |
| CN109234703A (en) * | 2018-11-27 | 2019-01-18 | 湖南顶立科技有限公司 | A kind of gas-phase deposition system |
| CN111363544A (en) * | 2018-12-26 | 2020-07-03 | 中国科学院物理研究所 | Phosphorus-like electron-doped hexagonal boron nitride and preparation method thereof |
| CN115968361A (en) * | 2020-08-21 | 2023-04-14 | 赛峰航空陶瓷技术公司 | Method for depositing a coating on a line in a microwave field |
| CN117089825A (en) * | 2023-06-01 | 2023-11-21 | 无锡松煜科技有限公司 | Plating chamber with uniform fluid distribution and plating method |
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Application publication date: 20160203 |